Methods for extracting low molecular weight components from polyesters

Abstract

The invention relates to a method for removing low molecular weight components from polyesters and to a polyester with low polydispersity and a low proportion of low molecular weight components.

Description

[0001] The present invention relates to a method for extracting low-molecular-weight components from polyesters. Furthermore, the present invention relates to a polyester with low polydispersity and a low mass fraction of low-molecular-weight components. Technical background of the invention

[0002] Polybutylene succinate (PBS) is a copolymer of the monomers succinic acid and 1,4-butanediol. Polybutylene succinate belongs to the group of linear aliphatic polyesters.

[0003] Polyesters are polymers whose monomers are linked via ester functions, which in turn form the main chain.

[0004] Polyesters are usually produced by polymerization or polycondensation. Both methods involve linking monomers to form polymer chains of varying lengths. These polymer chains can be linear, branched, or circular. PBS is typically produced by polycondensation. Depending on how the mean chain length is adjusted, the synthesis yields a polymer with varying weight-average molecular weights (Mv). w ).

[0005] Regardless of the weight-mean molecular weight (M w ) the polycondensate still contains monomers and low molecular weight condensation products - linear as well as ring-shaped - after polymerization, with a mass average molar mass (Mw) of ≤ 2,000 / mol.

[0006] This phenomenon is also known from other polycondensates such as polyamide 6.

[0007] The presence of low-molecular-weight components undesirably alters the properties of pure PBS. They act as plasticizers, which can affect the modulus of elasticity (Young's modulus) and the limiting bending stress. Furthermore, over time, the low-molecular-weight compounds (extract) tend to leach out of the polybutylene succinate and form a coating on the material surface. The greasy feel and the visual impairment of glossy or colored components reduce the marketability of extract-containing polybutylene succinates, so that their use today is limited, e.g., for components in non-visible areas. These impairments are also known, for example, from polyamide 6.

[0008] The crude polymer contains approximately 2% or more by weight of components with a mass average molar mass (Mw) of ≤ 2,000 g / mol.

[0009] For widespread use of the polymer, these components would need to be separated by extraction. Various methods can be used for polymer extraction, such as Soxhlet extraction, solid-liquid extraction with solvents and solvent mixtures, supercritical fluid extraction, and ultrasonic extraction.

[0010] Preferably, in the prior art, a portion of the extract is separated from the crude polymer after polymerization with a mixture of water and ethanol and / or isopropanol.

[0011] However, previously known methods are insufficient, as the products obtained continue to show the formation of a coating (streaks) shortly after processing.

[0012] It has now been surprisingly discovered that non-aromatic, organic solvents selected from the group consisting of ethers, ketones, and mixtures thereof are particularly well suited as extraction agents. This allows the majority of the low-molecular-weight components to be extracted from the polyesters, thereby preventing striae formation in polyester components. Description of the invention

[0013] The present invention relates to a method for the extraction of low molecular weight components from polyesters, characterized in that the method comprises the steps i) Presentation of a solid polyester-containing phase ii) Presentation of a liquid extraction solvent phase iii) bringing the solid polyester-containing phase into contact with the liquid extraction solvent phase, includes characterized by the fact that - the liquid extraction solvent phase comprises a non-aromatic organic solvent, wherein the non-aromatic organic solvent is selected from the group consisting of ethers, ketones and mixtures thereof, and - the solid polyester-containing phase contains a polyester which was produced from dicarboxylic acid monomers and diol monomers.

[0014] As mentioned above, in the inventive process the solid polyester-containing phase contains a polyester which was produced from dicarboxylic acid monomers and diol monomers.

[0015] The dicarboxylic acid monomers are preferably selected from the group consisting of alkane dicarboxylic acids, alkene dicarboxylic acids, and mixtures thereof; more preferably from oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, maleic acid, and furmaric acid; and more preferably from succinic acid, maleic acid, and mixtures thereof. In this disclosure, "mixtures of monomers" means that different types of monomers may be present. For example, a mixture of succinic acid and maleic acid monomers can be used in the polycondensation with a diol.

[0016] The diol monomers are preferably selected from the group consisting of 1,2 ethanediol, 1,3 propanediol, 1,4 butanediol, 1,5 pentanediol and 1,6 hexanediol; the diol monomer 1,4 butanediol is more preferred.

[0017] Accordingly, the polyester can be composed of various dicarboxylic acid subunits and diol subunits. Preferably, the polyester is a polybutylene succinate made from succinic acid and 1,4-butanediol monomers, a polyester made from succinic acid, maleic acid and 1,4-butanediol monomers, or mixtures thereof.

[0018] The solid polyester-containing phase may contain other components besides polyester.

[0019] Preferably, the solid polyester-containing phase contains the polyester in an amount in the range of 20 to 100 wt.%, more preferably 40 to 100 wt.%, and even more preferably 50 to 100 wt.%, based on the total weight of the solid polyester-containing phase.

[0020] Other possible components of the solid polyester-containing phase, which are also typically found in polyester components, include, for example, soapstone flour or polylactide.

[0021] Preferably, the solid polyester-containing phase is in pellet form. The liquid extraction solvent phase comprises a non-aromatic organic solvent, wherein the non-aromatic organic solvent is selected from the group consisting of ethers, ketones, and mixtures thereof.

[0022] Preferably, the non-aromatic organic solvent is selected from the group consisting of cyclic ethers, ketones and mixtures thereof; more preferably, the non-aromatic organic solvent is selected from the group consisting of tetrahydrofuran, acetone, or mixtures thereof; even more preferably, the non-aromatic organic solvent is tetrahydrofuran or acetone.

[0023] Preferably, the liquid extraction phase contains the non-aromatic, organic solvent in an amount in the range of 20 to 100 wt.%, more preferably 25 to 100 wt.%, based on the total weight of the liquid extraction phase.

[0024] In addition to the non-aromatic, organic solvent, the liquid extraction solvent phase may contain other inorganic solvents.

[0025] In a preferred embodiment, the liquid extraction agent phase contains tetrahydrofuran (THF) and water. More preferably, the liquid extraction agent phase contains THF and water with a weight ratio of THF to water in the range of 1:10 to 7:10, and even more preferably from 2:10 to 5:10. It is preferred that in step iii) the solid polyester-containing phase and the liquid extraction agent phase undergo movement relative to each other.

[0026] Preferred methods for step iii) are Soxhlet extraction, stirred solid-liquid extraction or migration of the extraction solvent front through a fixed bed of the solid polyester-containing phase.

[0027] Preferably, the weight ratio of the polyester-containing phase to the extraction agent phase in stirred solid-liquid extraction is in the range of 1:1 to 1:100, more preferably from 1:15 to 1:75, and even more preferably from 1:18 to 1:60.

[0028] Step iii) is preferably carried out for a period in the range of 0.1 to 72 h, more preferably from 1 to 36 h, and even more preferably from 2 to 30 h.

[0029] In step iii) the temperature is preferably in a range of 30 to 80 °C, more preferably from 45 to 60 °C.

[0030] Furthermore, the procedure preferably includes the following steps iv) Separation of the solid polyester-containing phase from the liquid extraction solvent phase, and v) Drying the solid polyester-containing phase, yielding a polyester-containing solid with low extractable content.

[0031] Preferably in step v) the extracted polyester-containing solid is dried at elevated temperatures between 30 and 100 °C and an absolute pressure in the range of 0.1 to 100 mbar until constant weight is achieved.

[0032] The non-aromatic organic solvent of the liquid extraction phase, which contains the extracted low molecular weight components of the polyester after the extraction process, can be recovered by distillation, preferably by distillation at reduced pressure.

[0033] The polyester obtained by the process according to the invention contains a significantly reduced weight fraction of low molecular weight components. Accordingly, the extracted polyester has a weight fraction of low molecular weight components, such as polycondensation products and monomers, with a mass average molar mass (Mw) of ≤ 2,000 g / mol, of less than 1 wt.%, preferably in the range of 0.01 wt.% to 0.5 wt.%, based on the total mass of the polyester.

[0034] Due to the reduced proportion of low-molecular-weight components, the polyester according to the invention has a lower polydispersity (M w / M n ).

[0035] The polyester according to the invention preferably has a polydispersity (M w / M n ), determined by GPC in the range of 2.0 to 5.0, more preferably from 3.0 to 4.5. Experimental part: Determination of the Rf value of the components of PBS in solvents

[0036] The Rf The elution number was determined using thin-layer chromatography in a setup as described in Fig. Figure 1 shows how the Rc is determined. For thin-layer chromatography (TLC), the stationary phase support (SiO2 or Al2O3) is applied as a thin layer of uniform thickness to a flat, degreased plate (3). These oxides contain up to 15% binder (usually gypsum) to stabilize the layer. For the determination of the Rc f -Values ​​in the present disclosure were obtained using commercially available, pre-coated DC films ALUGRAM Xtra SIL G / UV254 from Macherey-Nagel.

[0037] Thin-layer chromatography was performed at room temperature (25 °C±2 °C). Preparing the plate (3)

[0038] The crude polymer, the extracted polymer (raffinate), and the mixture of extracted components (extract) were compared. These had to be positioned on a horizontal line (starting line) at a uniform distance of approximately 10–12 mm from the lower edge of the plate. This starting line was drawn with a pencil. The substances to be tested were applied to this line in dissolved form. A 0.5 wt% PBS solution in chloroform was used. Pre-made microcapillaries were used for application; the solution was allowed to penetrate the capillaries. When the filled capillary was placed perpendicularly onto the layer, the solution flowed out again. The diameter of the resulting spots was 1–2 mm. The distances between the spots were > 5 mm, and the distances from the lateral edges of the plate were > 8 mm. Preparation of the DC chamber (2)

[0039] Before the plate with the samples was placed in the TLC chamber, the solvent or solvent mixture to be analyzed was introduced into the chamber (2) so that a solvent level (4) of approximately 7 mm formed in the chamber (2). The chamber (2) was then covered with a lid (1) and left to stand for approximately 5 minutes to allow the atmosphere inside the chamber to become saturated with solvent. Thin-layer chromatography process

[0040] After the substance spots had dried, the plate (3) was placed in the coverable chamber (2) containing the solvent or solvent mixture (4). Due to capillary action, the mobile phase rose against gravity in the TLC plate. Once the planned height was reached (approximately 1 cm from the top of the plate), the TLC plate was removed from the chamber, the mobile phase front was immediately marked (pencil line), and the plate was dried in air (fume hood). DC evaluation

[0041] The disk was evaluated by comparison with an authentic connection running on the same disk and by calculating the R F -values. The R F The R-value is the ratio of the distance traveled by the substance to the distance between the starting line and the front of the solvent. F The -value is a characteristic quantity for each compound in this particular separation system (solvent composition, temperature, solvent ratios to all components). Gel permeation chromatography

[0042] The polyesters used were analyzed before and after the extraction process by gel permeation chromatography (GPC) according to DIN EN ISO 13885-1. An Agilent Polymer Laboratories system with the following equipment was used: - PLgel 10 µm pre-column - 3 x PLgel 20 µm Mixed-A, 7.5 mm ID x 300 mm, 2,000 - 40,000,000 g / mol - Device control, data acquisition and processing with the Empower 3 FR5 software (Waters)

[0043] The following GPC conditions have been set: - Eluent: TCM (trichloromethane) - Flow rate: 1 mL / min - Column oven temperature: 25 °C - Injection volume: 100 µL (22 °C) - Sample concentration: 5 mg / ml - Detector: RI 30 °C Sample preparation

[0044] 20 mg of the samples were dissolved in 4 ml of eluent by gentle shaking for 20 h at room temperature. The solutions were clear, and the samples were completely dissolved. The solutions were filtered through 1 µm PTFE membranes and injected directly into the GPC. GPC measurements were then performed. PBS starting polymers used PAZ 20: PBS with a number-average molar mass (M n ) of 22 kg / mol, a mass average of the molar mass (M w) of 173 kg / mol, and a polydispersity (M w / M n ) of 7.9. The mass fraction of low molecular weight condensation products with a mass average of molar mass (M w ) of ≤ 2,000 g / mol in the commercial PBS was 1.86 wt.%, determined by GPC and confirmed by mass balance, sample and extract. PAZ 29: PBS with a number-average molar mass (M n ) of 22 kg / mol, a mass average of the molar mass (M w ) of 173 kg / mol, and a polydispersity (M w / M n ) of 7.9. The mass fraction of low molecular weight condensation products with a mass average of molar mass (M w ) of ≤ 2,000 g / mol in the commercial PBS was 1.84 wt.%, determined by GPC and confirmed by mass balance, sample and extract. FZ71: Commercial PBS from Mitsubishi Chemical Performance Polymers (MCPP) with a number-average molar mass (M n ) of 29 kg / mol, a mass average of the molar mass (M w) of 141 kg / mol, and a polydispersity (M w / M n ) of 4.9. The mass fraction of low molecular weight condensation products with a mass average of the molar mass (M w ) of ≤ 2,000 g / mol in the commercial PBS was 1.12 wt.%, determined by GPC and confirmed by mass balance, sample and extract. FZ91: Commercial PBS from Mitsubishi Chemical Performance Polymers (MCPP) with a number-average molar mass (M n ) of 39 kg / mol, a mass average of the molar mass (M w ) of 199 kg / mol, and a polydispersity (M w / M n ) of 5.1, determined by GPC. The mass fraction of low molecular weight condensation products with a mass average of the molar mass (M w ) of ≤ 2,000 g / mol in the commercial PBS was 1.11 wt.%, determined by GPC and confirmed by mass balance, sample and extract. Example according to the invention 1

[0045] 10,000 g of polybutylene succinate (PAZ 20) was extracted using a Soxhlet extraction process for 24 h with acetone as the extraction solvent at a temperature of 56 °C. The extraction solvent was then concentrated using a rotary evaporator at 56 °C and a final vacuum of 80 mbar absolute pressure. The resulting extract was dried in a vacuum drying oven at < 10 mbar absolute pressure for a further 10 h until constant weight was achieved. The extracted granules were then dried in a vacuum drying oven at a temperature of 40 °C and a final pressure of < 10 mbar absolute pressure for 24 h until constant weight was achieved. The mass of the extracted polybutylene succinate PBS ex The weight after extraction was 9.807 g. The mass of the extract after drying was 0.193 g. To rule out degradation of the polybutylene succinate by extraction, the polymer samples before and after extraction, as well as the extract, were analyzed by gel permeation chromatography (GPC). Fig. The graphical evaluation of the obtained data is shown. The mass average of the molar mass (M) w ) of the PBS ex was 172 kg / mol and the polydispersity (M w / M n ) decreased to 4.0. The extracted polybutylene succinate PBS ex After 60 days of storage at 40 °C, no striae formed on its surface. 96.3 wt% of the initial amount of the extraction solvent was recovered after drying the polymer and the extract. Examples according to the invention 2a-2d

[0046] Four extractions, each using 10,000 g of polybutylene succinate (PAZ20), were carried out using a stirred solid-liquid extraction process for 1, 3, 6, and 10 h at a temperature of 50 °C. The extraction solvent consisted of 30 wt.% tetrahydrofuran and 70 wt.% water. The weight ratio of polymer to extraction solvent mixture was 1:20 in each case. After the extraction time, granules and extracts were separated and dried as in Example 1. The masses of the extracted polybutylene succinate PBS were determined by the following formulas: ex The masses after extraction were 9.945 g, 9.890 g, 9.815 g, and 9.808 g. The extract masses after drying were 0.055 g, 0.110 g, 0.185 g, and 0.192 g. The mean masses of the molar mass (M w ) of the respective PBS ex (2a)-PBS ex (2d) After extraction, the concentrations were 173, 172, 173 and 172 kg / mol and the polydispersities were 7.2, 7.0, 5.9, and 4.0 (see Table 1). The PBS extracted for 1, 3 and 6 h ex (2a)-PBS ex(2c) showed striae formation on the surfaces after 4 to 12 days of storage at 40 °C. The PBS extracted for 10 h ex (2d) showed no striae formation after 60 days at 40 °C. After drying the polymer and the extract, 96.1 wt.%, 95.8 wt.%, 95.7 wt.% and 96.0 wt.% of the initial quantity of the extraction solvent mixture used could be recovered. Table 1: Properties of the polyesters of examples 2a-2d Example PAZ20 2a 2b 2c 2d M w [kg / mol] 173 173 173 173 172 M w / M n 7,9 7,2 7,0 5,9 4,0 PBS:LM - 1:20 1:20 1:20 1:20 Duration [h] - 1 3 6 10 m(extract) [g] - 0,055 0,110 0,185 0,192 Streaks 40°C J J J J N Examples according to the invention 3a-3e

[0047] Five extractions (3a-3e), each using 10,000 g of polybutylene succinate (PAZ20), were carried out using a stirred solid-liquid extraction for 3 h at a temperature of 50 °C. The extraction solvent consisted of 30 wt.% tetrahydrofuran and 70 wt.% water. The weight ratio of polymer to extraction solvent mixture was 1:2, 1:5, 1:10, 1:20, and 1:50. After the extraction time, granules and extracts were separated and dried as in Example 1. The masses of the PBS ex The masses after extraction were 9.980 g, 9.950 g, 9.925 g, 9.890 g, and 9.807 g. The extract masses after drying were 0.020 g, 0.050 g, 0.075 g, 0.110 g, and 0.193 g. The mass means of the molar mass (M w ) of the respective PBS ex After extraction, the precipitates were 173, 173, 173, 172, and 171 kg / mol, and the polydispersities decreased to 7.8, 7.2, 6.9, 5.3, and 4.0 (see Table 2). The PBS extracted at weight ratios of 1:2 to 1:20ex (3a)-PBS ex (3d) showed schlieren formation on the surfaces of the PBS obtained with a weight ratio of 1:50 after storage at 40 °C for 2 to 10 days. ex (3e) showed no striae formation after 60 days. After drying the polymer and the extract, 95.4 wt.%, 95.8 wt.%, 95.8 wt.%, 96.1 wt.% and 96.0 wt.% of the initial quantity of the extraction solvent mixture used could be recovered. Table 2: Properties of the polyesters of examples 3a-3e Example PAZ20 3a 3b 3c 3d 3e M w [kg / mol] 173 173 173 173 172 171 M w / M n 7,9 7,8 7,2 6,9 5,3 4,0 PBS:LM - 1:2 1:5 1:10 1:20 1:50 Duration [h] - 3 3 3 3 3 m(extract) [g] - 0,02 0,05 0,075 0,110 0,193 Examples 4 and 5 according to the invention

[0048] 5,000 g each of a polybutylene succinate (Mitsubishi FZ71 for Example 4 and FZ91 for Example 5, both copolymers of succinic acid, 1,4-butanediol, and maleic acid) were extracted in a fixed bed with a moving extraction solvent front for 12 h using acetone as the extraction solvent at a temperature of 50 °C. The extraction solvent was then concentrated on a rotary evaporator at 56 °C and a final vacuum of 80 mbar absolute pressure. The resulting extract was dried in a vacuum drying oven at < 10 mbar absolute pressure for a further 10 h until constant weight was achieved. The extracted granules were then dried in a vacuum drying oven at a temperature of 40 °C and a final pressure of < 10 mbar absolute pressure for 24 h until constant weight was achieved. The masses of the resulting PBS ex (4) and PBS ex (5) were 4962.8 g and 4967.5 g. The extract masses after drying were 37.2 g and 32.6 g. The mass mean of the molar mass (M w ) for PBSex (4) was 142 kg / mol and the polydispersity decreased to 4.0. The mass average of the molar mass (M w ) for PBS ex (5) was 198 kg / mol and the polydispersity decreased to 4.1. The extracted polybutylene succinate PBS ex (4) and PBS ex (5) showed no striae formation on the surface after 60 days of storage at 40 °C. The unextracted control samples of FZ71 and FZ91 showed striae formation after 3 to 5 days at 40 °C. The extraction solvent used could not be detected after drying the PBS. ex and of the extract 98.3 wt.% and 98.2 wt.% of the initial quantity are recovered. Example 6 according to the invention (scale increase)

[0049] 96.3 kg of polybutylene succinate (PAZ 29) were extracted in a fixed bed with a moving extraction solvent front for 12 h using acetone as the extraction solvent at a temperature of 50 °C. The extraction solvent was then concentrated in an evaporator at 56 °C and a final vacuum of 80 mbar absolute pressure. The resulting extract was dried in a vacuum drying oven at less than 10 mbar absolute pressure for a further 20 h until constant weight was achieved. The extracted granules were then dried in a gyratory dryer at a temperature of 80 °C and a final pressure of < 10 mbar absolute pressure for 24 h until constant weight was achieved. The mass of the extracted polybutylene succinate PBS ex (6) was 94.4 kg after extraction. The extract mass after drying was 1.9 kg. The mass average of the molar mass (M w ) for PBS ex (6) was 205 kg / mol and the polydispersity decreased to 3.05. The extracted polybutylene succinate PBS ex(6) showed no streaking on the surface after 60 days of storage at 40 °C. 99.6 wt% of the extraction solvent used was recovered after drying the polymer and the extract. Comparative example 7

[0050] 10,000 g of polybutylene succinate (PAZ20) was extracted by stirred solid-liquid extraction for 10 h at a temperature of 56 °C. The extraction solvent consisted of 10 wt% ethanol and 90 wt% water. The weight ratio of polymer to extraction solvent mixture was 1:50. After the extraction time, the extraction solvent and extract were separated from the extracted polymer by filtration through a G3 frit. Subsequently, the extract and polymer granules were dried as described in Example 1. The mass of the extracted polybutylene succinate (PBS) was... ex(7) was 9.903 g after extraction. The extract mass after drying was 0.097 g. The mass average of the molar mass (M w ) for PBS ex (7) at 163 kg / mol and the polydispersity decreased to 6.1. The extracted polybutylene succinate (PAZ20) shows distinct streaking on its surface after 3 days of storage at 40 °C. After drying the polymer and the extract, 96.5 wt% of the initial amount of the extraction solvent mixture used could be recovered. Testing of oligomer regression

[0051] The extracted PBS produced under examples 1 to 5 ex The samples were tested for oligomer regeneration. For this purpose, the samples were tempered for 24 hours at 80 °C, 40 minutes at 150 °C, and 40 minutes at 200 °C, quenched, dried, and then measured. Fig. 4 and Fig.Figure 5 shows that no regression can be observed under the investigated conditions and only a slight reduction in molecular weight can be seen in the 200 °C samples.

Claims

[1] A method for the extraction of low molecular weight components from polyesters, characterized by that the procedure includes the steps i) Presentation of a solid polyester-containing phase ii) Presentation of a liquid extraction solvent phase iii) bringing the solid polyester-containing phase into contact with the liquid extraction solvent phase, includes, characterized by , that - the liquid extraction solvent phase comprises a non-aromatic organic solvent, wherein the non-aromatic organic solvent is selected from the group consisting of ethers, ketones and mixtures thereof, and - the solid polyester-containing phase contains a polyester which was produced from dicarboxylic acid monomers and diol monomers. [2] The method according to claim 1, characterized bythat the dicarboxylic acid monomers are selected from the group consisting of alkane dicarboxylic acids, alkene dicarboxylic acids, and mixtures thereof, preferably from oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, maleic acid and furmaric acid, preferably selected from succinic acid, maleic acid and mixtures thereof. [3] The method according to one of claims 1 or 2, characterized by , that the diol monomers are selected from the group consisting of 1,2 ethanediol, 1,3 propanediol, 1,4 butanediol, 1,5 pentanediol and 1,6 hexanediol, preferably the diol monomer 1,4 butanediol. [4] The method according to any of the preceding claims, characterized by , that the non-aromatic organic solvent is selected from the group consisting of ketones, cyclic ethers and mixtures thereof, preferably the non-aromatic organic solvent is tetrahydrofuran or acetone. [5] The method according to any of the preceding claims, characterized by , that the low molecular weight components of the polyester-containing phase have an R f -value of more than 0.2, determined by thin-layer chromatography with the liquid extraction phase as the mobile phase, and the high molecular weight components of the polyester-containing phase have an R f -value of less than 0.

05. [6] The method according to any of the preceding claims, characterized by , that in step iii) the solid polyester-containing phase and the liquid extraction solvent phase undergo a movement relative to each other, wherein the relative movement is preferably caused by a Soxhlet extraction, a stirred solid-liquid extraction or by migration of the extraction solvent front through a fixed bed of the solid polyester-containing phase. [7] The method according to any of the preceding claims, characterized by that the procedure includes the steps iv) Separation of the solid polyester-containing phase from the liquid extraction solvent phase, and v) Drying the solid polyester-containing phase, yielding a polyester-containing solid with low extractable content. [8] The method according to any of the preceding claims, characterized by , that step iii) is carried out for a period in the range of 0.1 to 72 h, preferably from 1 to 36 h, more preferably from 2 to 30 h. [9] The method according to any of the preceding claims, characterized by , that step iii) is carried out at a temperature in the range of 0 to 100 °C, preferably from 30 to 80 °C, more preferably from 45 to 60 °C. [10] The method according to any of the preceding claims, characterized bythat the solid polyester-containing phase contains the polyester in an amount in the range of 20 to 100 wt.%, preferably 40 to 100 wt.%, more preferably 50 to 100 wt.%, based on the total weight of the solid polyester-containing phase. [11] The method according to any of the preceding claims, characterized by that the liquid extraction phase contains the non-aromatic organic solvent in an amount in the range of 20 to 100 wt.%, preferably 25 to 100 wt.%, based on the total weight of the liquid extraction phase. [12] A polyester which was produced from dicarboxylic acid monomers and diol monomers, characterized by that the polyester has a polydispersity (M w / M n), determined by GPC in the range of 2.0 to 5.0, preferably 3.0 to 4.5, and the weight fraction of low molecular weight polycondensation products with a mass average molar mass (Mw) of ≤ 2,000 g / mol and monomers with a mass average molar mass (Mw) of ≤ 2,000 g / mol together is less than 1 wt.%, preferably ≤ 0.5 wt.%, more preferably in a range of 0.01 wt.% to 0.5 wt.%, based on the total mass of the polyester.

Images