TW201035159A - Process for purifying semiconductive polymers - Google Patents

Abstract

The invention relates to a novel process for purifying semicondctive polymers by contacting with an ion exchanger, and to the polymers of high purity obtained from the process.

Description

201035159 VI. Description of the invention: [Technical field to which the invention pertains] The present invention relates to a high-purity H-guided method for the leakage of the ion-hull polymer (four) method [Prior Art] Ο Ο Conductor in a half-multiple case High Purity - The semi-t-body "recorded product or semi-finished product meets the requirements for subsequent end use. Such products made of semiconducting polymers and r are printed on the surface with such inks and "circuitry; in the case of semiconductor polymers, sufficient purity is particularly relevant for metal or semi-metal contamination, The semiconductor characteristics of the object can be adversely affected. You u ^ -V ^ ^ W Λ , 扪 扪 曰 曰 曰 曰 曰 曰 曰 ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ ¥ A transistor element is used as an electrical conductor that no longer performs ageing. More specifically, the maximum metal and/or semi-metal contamination is necessary to be $卯m and lower, * which may have to be met for use in high quality products. 2004 106403 A1 discloses a method for preparing a relatively pure semiconducting polymer, characterized in that a first-stage semiconductor polymer is formed in a spray and is contacted with water containing a metal ion-intercalating agent by dissolving in another spray. It is then separated from the solvent to release the impurities. 3 201035159 In the town of WO 2004 106403 A1 - Purchasing mountain organic solvent in the protective gas under the protective gas is better to dissolve in the suitable metal ion complexing agent is a variety of acetic acid in the water phase presence. Wang Wuqi in W〇 2004 leg 03αι$, followed by solvent phase and water phase magic mode, intensive contact. It is disclosed herein that the simple, shaking extraction, for: is not sufficient for purification and must be mixed with, in place of, intensive mechanical extraction. The small day " therefore disclosed methods for purifying semiconducting polymers have disadvantages in that they are extremely costly and inconvenient and harmful to the environment. After the contamination of the disclosed purification process, the special organic imitation must be re-used with special treatments or _ must be converted to high cost and money. In addition, taking a small amount of the purified material for use in the process of preparing a semiconducting polymer has the same disadvantages. It also raises the problem of the degree of reuse of water C, because according to the basic force j '", the law excludes the absorption of water phase - the specific amount of gas imitation, which will cause the above problem when operating this phase 'and because it does not reveal After the desired mismatch, the metal ion intercalating agents can be used again to take metal ions. The use of the ion exchange material is not disclosed. The ion exchange material makes the purification of the semi-fourth polymer system problematic because it is in principle _ The sequence of the inspection-series limit _ sub-exchange material is inclined to avoid the H, the influence is well known. /, Unfavorable these boundary conditions are, for example, the reaction zone in the reaction zone 201035159 where ion exchange materials are present should be Keep the minimum value to *, and take the force on the resin on the exchange of the scorpion. Because of the high pressure drop of the semiconducting polymer, it is transmitted to the right habitat, the sardine, the threshold and thus the formation. At low 4', these methods have a significant limitation on the temperature of the multi-material mm (4), in which the chemical structure of Xu Xi (4) is damaged at a high s5 (temperature of rc). Material, according to bribe Lion 9 should not only be (4) up to Q.5 ah 4 New Year's poems. And Post 2 and other oxidizing substances should be present in the starting material with no more than 1ppm to prevent oxidative damage of ion exchange materials. = "sample" should be removed from the silk towel in advance to remove irreversible Wei materials such as ions | surfactants or metal complexes and clear particles or organic by-products - because these materials also reverse the material exchange materials and Thus, the purification properties of the ion exchange material are completely lost. A preferred method for purifying the semiconducting polymer is disclosed in WO 〇 2005 041321 A1. In the method disclosed herein, the shilling dilute semiconductor polymer is subjected to ultrafiltration treatment to remove Non-ionic impurities of a particular size. In this context, the size of the impurities that can be removed is affected by the type of membrane used in the ultrafiltration. In another procedure, the ionic impurities of the above-mentioned metal or semi-metal in salt form are then removed. It reveals that the maximum proportion of impurities in the disclosed product can be 90 ppm when diluted to 2% by weight. The ratio of cation and anion impurities in each case Up to 30 ppm. The methods disclosed for the removal of anionic and cationic impurities are filtration, column filtration (adsorption), dialysis, chromatography and centrifugation. Another disclosed 5 201035159 is a chromatographic ion exchange chromatography. However, it is preferred to use an ion exchanger and a cation exchanger for the purification of the cation exchanger. If the cation is used according to W0, the cation can be purified in a particularly simple and rapid manner. The exchanger has (4) and weak acid properties = ion exchanger, which is made of polystyrene, polyf-propyl-based or polypropylene-based, _c〇〇m -N=(CH2C〇〇)2M ( Wherein Μ is preferably a hydrogen atom group, or one, it also reveals a positive ion exchange agent for a heavy metal material. The disclosed anion exchangers have anionic crosslinks which are extremely strong to the weakest test properties, especially those having a four-grade or tertiary amine on the polystyrene and polypropylene bases. In the disclosed method, the purification of the anion and cation impurities is removed, and the first filter having an anion exchanger having a quaternary (four) phenol on the styrene is always prepared, and then the polystyrene-containing and -S〇3H are used. The cations are _ m. The disclosed ranks are two, four or six in each case. According to this disclosure, the best results are obtained when six filter stages are used for each purification. It is additionally disclosed that it must be diluted in a large amount of 1.20 before being specifically purified by an ion exchanger. This is obviously to achieve a reduced viscosity to avoid the above problems associated with the use of ion exchange materials. The method disclosed in WO 2005 041321 A1 has disadvantages in that the metal (cationic impurity) is lower than 201035159 5pprn only when six filters are connected in series and pre-dilution of the above 2% by weight semiconductor polymer solution has been carried out. The highest purity available. Further, the content of the metal to be transferred in the towel is based on the content of the metal in the polymerization of the cover containing the 2% by weight of the semiconductive compound, wherein the metal content is about 25 Å. This department can have disadvantages.持续 / ^ According to the shortcomings of the prior art, the continuing object and object of the present invention is to provide a method for purifying a semiconducting polymer ☆ which can remove metals and/or semimetals from a semiconducting polymer in a simple process Ο g-\ Can be incorporated into 1 continuous manufacturing process. /, [Summary of the Invention] Surprisingly, it has been found that the object is achieved by a method of purifying a semiconductor, characterized in that a solution containing a semiconductor polymer having a content of from 丨 to 3/r/°^ is passed through - a purification zone containing an ion exchange resin, wherein the ion exchange resin is contained

The polymer contains a sulfonic acid group. K. The semiconducting polymer to which the present invention relates is a polymer comprising at least a k-single unit of sigma, phenanthrene, aniline or pyrene, preferably containing at least one thiophene. More preferably, the monomer unit of the base monomer has at least one monomer unit of 3-hexyl σ-cephen. The semiconductor polymers which have been purified by the process according to the invention can be obtained by the method of WO 2008 080513 Α1. 1~ In a preferred embodiment, the process according to the invention is characterized by comprising 7 201035159 comprising a semiconductor polymer in an amount of from 1 to 3% by weight and the solution supplied to the process comprising a metal/semimetal content of more than 1000 ppm. Surprisingly, it has been found that the sulfonic acid group on the polystyrene-based copolymer can directly make the highly concentrated semiconductor polymer solution in an amount of from 1 to 3% by weight free of metal/semimetal, and to make it a solution. The content is less than 1 ppm after the procedure. More specifically, this does not detect the adhesion of the ion exchange resin to the semiconducting polymer during the process. Preferred ion exchange resins containing a sulfonic acid group on the polystyrene-containing copolymer are ion exchange resins containing a divinylphenyl group in addition to the polystyrene group. The test of the good ion father to change the resin for them can generally be Lewa 8spη2

The trade names of LeWatit® K2621 and Lewatit® K2629. In addition to the particularly advantageous properties that have just been omitted for the purpose of omitting dilution by removing metal and/or semi-metals, the present invention compares. The resin and the ionic parent are replaced by a resin which is also advantageously used in the process according to the invention because it can be used at temperatures up to 1% ° C to allow direct heat flow from the preparation of the semiconducting polymer. . Therefore, it is preferred to carry out the invention in a purification zone at a temperature of 8 (rc to !20t). It is high in size (4) because it is high enough to significantly increase the solubility of the bulk polymer in the spray while at the same time significantly reducing The viscosity of a solution containing a semiconductor polymer containing lining:,, and 1 to 3% by weight. The solvent related to the present invention means that all of the liquid is at a temperature exceeding 120 t and the semiconductor polymer can be at least 1% by weight. Proportion 201035159 Dissolved substance or mixture of substances. The process according to the invention is generally carried out at a inlet pressure of the purification zone of 1.1 to 2.0 bar. Such pressures are particularly advantageous because of the preferred operation of the process according to the invention as disclosed above. The temperature and preferred solvent and solvent mixture disclosed hereinafter 'which results in a solvent or solvent mixture being a liquid and having a lower viscosity than the procedure of water. Similarly, the pressure can be passed through.

The purification zone' is characterized by a high pressure drop depending on the concentration of the semiconducting polymer in the solution. In general, the process according to the invention is not limited in terms of solvent availability. The completeness of the procedure is only the solubility of the at least 丨% by weight of the semiconducting polymer at the temperature and pressure at which the procedure is carried out and in fact the solvents are not solvents for the ion exchange resin and the solvents do not contain any Water is necessary for the oxidative corrosion of the ion exchange material. _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ A compound containing an engraving group such as diethyl ether, oxane and tetrahydroindenyl dibutyl methyl ether, dibutyl ether, pentyl ether, methane (THF). In the method of the present invention, it is preferred to use a thiol-containing agent: a particularly preferred solvent is tetranitron. It is also possible to use a mixture of two classes of tetrahydrofuran = state, a mixture of grains. The especially good solvent mixture contains benzene. In general, the 'solvent or solvent mixture is determined according to the requirements of the manufacturing method 9 201035159' and is not disclosed herein as required by the purification method of the present invention. 〆 Therefore, the solvent or solvent mixture is generally selected such that the thiophene derivative or polymerization activity used prior to the addition of the coal during the manufacturing process has been present in dissolved form. Because relatively high concentrations of starting materials are generally required or preferred for this purpose, the requirements for the portion of the semiconducting polymer that is soluble in the solvent-forming roll mixture in the purification process disclosed herein are at least 1% by weight. Comply with the requirements of the program. For the purifications disclosed herein, in addition to the preferred tetrahydrofuran and preferred solvent mixtures containing tetrahydrofuran and toluene, it has been found that halogenated aliphatic hydrocarbons such as dichloromethane and gas imitation are particularly suitable. . Solvent mixtures containing tetrahydrofuran and methyl is particularly advantageous because of its combination of particularly advantageous properties. For example, tetrahydrofuran is compatible with water and methyl, making it useful as a co-solvent for water in solution without layer formation, and the viscosity of both solvents is lower than that of water, which is also an advantage. Therefore, the combination of the two solvents in the mixture is particularly advantageous for the methods disclosed herein. In view of the necessary preparation procedures carried out in advance, the fact that the method according to the invention is not limited by the solvent or solvent mixture is formed here to form another important advantage of the method according to the invention, since it can thus be integrated in a simple manner without the need for a preparation procedure. The intermediate stage between the purification process and the purification process is interlinked to the existing process for preparing semiconducting polymers. The ion exchange resin can be present in the purification zone in any geometric form. However, a bed of ion exchange resin particles is preferred. 2 Tetraic particles have an average diameter of 0.01 to 2 mm. Ion intersection 201035159 Finish: Single mode It: The particle size distribution of the other particularly good particle bed is substantially advantageous for the product relative = ^_ bed system, because this is in the particle The available surface = = the lower reaches the relative optimum. During the purification of the particles, "two two? = in purification, but in the present invention through the dissolution of the ruthenium polymer, the operation transport contains a semi-conducting economy. /, the energy consumption required for pumping makes this procedure change If the surface is not produced, the equivalent amount of ion exchange resin will no longer be obtained. The corresponding larger amount of ion exchange resin in the second reversible region will be left in a large proportion. = exchange capacity of the resin, which is at least economically disadvantageous, beneficial, "in some cases, if the ion exchange resin does not increase in the purification zone I, it can no longer achieve the purpose of purification. Purely completely complete The modal distribution is unfavorable because it does not produce any area of the region with relatively large particles in the flow or the ^. Because it is impossible to ensure that the semiconductor contains poly (in) and because it is unreachable or at least not = reliable purification of metals and/or semi-metals, which in this way produces different flow rates in the && domains. The particles of the ion exchange resin are additionally preferably porous. Many, the daughters have disadvantages due to the purification zone In the same volume for an ',, & for a larger surface area for purification by the above ion exchange resin may have ion exchange resin and # qe good soil properties, wherein the ⑽ exchange resin - as can be 201,035,159.

Trade names of Lewatit® SP112, Lewatit® K2621 and Lewatit® lC2629 were obtained. ° The process according to the invention can be carried out continuously or batchwise. With respect to the present invention, a batch refers to a solution containing a semiconductor polymer and the solution to be purified is introduced into a purification zone in which an ion exchange resin is present and the solution remains in the purification zone until the completion of the metal and/or semimetal. Purification or until the ion exchange resin essentially no longer has any other gold and/or semi-metal loading capacity. In a further development of the batch process according to the invention, the solution comprising the semiconducting polymer is separated from the ion exchange resin in a further step. When the purification is completed or the loading volume is reached, the separation is suitably achieved by a filtration method well known to those skilled in the art. The filtration equipment used herein can in principle be provided for all of the technical specific tables having sufficient filtration area for the required fineness of the filter medium. The other examples are a gas pump, a pressure filter, a pressure (four) and a belt filter. The filter or medium used may be a plastic or metal fabric, or a welded plate which is particularly commonly welded in the case of excessive exhaustion. ~ In the better specific performance of the separation, the reading is 100 microns. In this k-batch-man's advancement-step development, the present invention refers to this: A solution of the semiconducting polymer is introduced into the purification zone and retained in the 14 ion exchange resin, which is separated from the money in another step and discarded. The solution is retained in the pure 201035159 zone until the time of removal is determined by the same influencing parameters, similar to the residence time of the continuous feed as described below. Within the specific performance of the batch of the procedure, the degree of ion exchange resin is preferably greater than 6 / 8 liters, preferably greater than 120 grams / liter, and then the residence time is up to 4 hours, based on the volume of the solution containing the semiconducting polymer. Better than at least 6 hours. Ό € , these concentrations and preferred residence times lead to excellent purification results in accordance with the batch process of the present invention. Or 'in the order of the batch: the inevitable cash, the material exchange f is set to change with the presence of metal and / or semi-metal in the solution, ~ Tian" time is determined to be 6 hours, in the semiconductor Preferably, each gram of metal and/or semimetal in the polymerized trough is 2 () to 3: the exchange resin is present in the purification zone. The skilled person will see that this residence time and the amount of ion exchange 4 are related to each other. The upper occupation only constitutes - it is beneficial to the specific image of the ^ ^ to other specific performance, its cap contains semiconductor polymerization three liquid ^ change or change with its pollution, in the region that is conducive to shorter retention = = can be imagined High-volume ruthenium lyophilized. Conversely, for longer retention of a smaller amount of ion exchange resin, there may be a car lane. 1 The present invention, continuous effect means a conductor passing through the room according to the present invention. The residence time of the solution of the polymer in the purification zone is 曰3. After the solution is passed through the purification zone, the ion exchange resin is selected to be any storage capacity for other metals and/or semimetals, or ^: : 'The metal that has been selected to exceed the purification zone:: 1 Then exceed the maximum value. Dry main genus 13 201035159 fascination 2 / before the stagnation (4) and for the optional restrictions according to the invention. Instead, 'the skilled person in the individual case preparation i and with the ion exchange resin Depending on the nature of the change and the amount of ion exchange resin present, the purification process can be operated at the advantages described herein. The parameters of the ion exchange tree or the parameters of the preparation method that may affect the purification performance The specific surface area or desired throughput of the resin for the resin, which is known for the method of preparing the semiconducting polymer. _ Beginning with the preferred further development of the method shown herein is characterized by a content of 1 to A solution of 3 weights 4% of the semiconducting polymer passes through a first purification zone containing an ion exchange resin (wherein the ion exchange resin comprises a sulfonic acid group on the polystyrene containing copolymer) until the first purification zone The content of the metal and/or semimetal at the outlet reaches a threshold, and then the solution containing the semiconductor polymer in an amount of 丨 to 3% by weight passes through the first purification zone instead Waiting for the second purification zone and simultaneously exchanging or regenerating the ion exchange resin of the first purification zone. With respect to the present invention, the enthalpy value means that the metal and/or the semimetal may be present in the purification solution containing the semiconductor polymer. Maximum value. This is generally a good idea. However, the specific advantages of the method shown here can be utilized only on the assumption that this value is 1 ppm or less. Suitable for the determination of metals and / or semi-metals in purification Methods and apparatus for the amount of solution in the zone exit are well known to those skilled in the art. Non-exclusive examples include, for example, scattered light measurements and transmission measurements of light through the solution stream. Continued further development, retention 14 201035159 time is therefore measured by the above enthalpy. The ion exchange resin is also used to exchange the tree method by means of # 者 再生 再生 再生 再生 非 非 非 ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; ; The in-situ emission 'ion enthalpy exchange _ Japanese system exists in the purification zone in the form of a solid boring bed. ϋ ϋ Therefore, the above-mentioned ion exchange resin particles are well known for use in equipment for immobilizing such beds, or ions: it is well known in the art that it is monolithic or structured to fill in two. The present invention is additionally provided in the presence of polystyrene. The copolymer comprises a sulfhydryl ion exchange resin for the purification of metals and/or semimetals in a concentration of from 1 to 3 by weight of the polymer solution of the conductor. + Ion Che Chau's polystyrene-based copolymer contains two bases containing divinylphenyl sulfonium in the ^ ^ is particularly advantageous, because it has been found that these specific and reversing (four) days can also make The content is from 丨 to 3% by weight, and no metal or semi-metal is contained in the night, and no adhesion is detected between the ion exchange = body compound. The invention is described in detail below with reference to the examples and drawings. The ~, , ·, and the figures show a method of development according to a preferred further development for purifying a semiconducting polymer. Figure 1 shows the conditions of the first and second purification zones (R1, R2) at the time t1 when the two exchange zones of the sub-exchange resin (A) still have a full load. A solution comprising a semiconducting polymer and a contaminant in the form of a metal and/or a semi-metal (L) is supplied to the first purification zone (Rl). The purified solution is obtained without metal and/or semi-metal (L,). Figure lb shows the conditions of the first purification zone (Ri) after the ion exchange resin (A) is almost loaded with contaminants in the form of metals and/or semimetals and has reached a threshold value. This stream is transferred to the second reaction zone (R2) of the ion exchange resin which is still unloaded. Figure lc shows the conditions after the purification zone (r2) is at the time tptpti at which the ion exchange resin (A) is completely loaded with the contaminants in the form of metal and/or semimetal (L). The stream is returned to the first reaction zone (R!) of the ion-exchange resin which is again unloaded. Restart the program. EXAMPLES Example 1: Batch-purified polythiophene solution was used in the purification of a poly-3-alkyl-based α-cephene solution (hereinafter, a poly 17-secret solution, according to Example 1 of WO 2008 080513 Α1) In one experiment, 50 ml of a polythiophene solution containing 1.3% by weight of polythiophene and 22 mg/kg of nickel and 2150 mg/kg of magnesium dissolved in tetrahydrofuran was initially charged into the first vessel. Different masses of ion exchange resin (Lewatit® SP112) according to Table 1 were added to this solution and purified at room temperature (23 ° C) and shaken for 24 hours. After 24 hours, the ion exchange resin was removed by filtration through a metal mesh having a mesh size of 1 μm in each case. Samples were taken from the purified solution in each case and analyzed for magnesium and nickel contents. 16 201035159 When the metal and / or semi-metal content is less than ι / kg, before the procedure and according to the data in Table 1 (and Tables 2 and 3 below) is similar to DIN EN ISO 11885 ICP-OES (induction Coupled plasma-light emission spectroscopy; instrument · Perkin Elmer Optima 3300XL) after microwave digestion (DIN ΕΝ 14084) or similar to DIN ΕΝ ISO 172994-2 by ICP-MS (inductive hybrid plasma-proton spectroscopy; instrument : Thermo Element II) Determination of the above listed nickel and magnesium contents in solution. Ο Ο Table 1: Experimental data according to Example 1 #Ion exchange resin mass [g] Purified Mg content [mg/kg] Purified Ni content [亳克/公斤1 1 0.5 850 16 2 1 460 12 3 2 180 5 4 2.5 <0.1 <1.0 5 3 0.013 --- 0.055 • ·—— a 隹1: When using 25 g of ion exchange resin in the solution at temperature and ==5 () ml, according to this The Sheming purification method can reduce the content of tilting and nickel to i mg / liter. The mass of the above-mentioned ion exchange resin is ML) and the thiophene solution of the metal and / 疋 ( ( 〇 〇 〇 〇 〇 〇 《 《 《 《 《 《 《 《 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩 吩Ion exchange m and metal/half gold. .g Table 1 (and the following list 3) The age of the symbol, such as this, because of the experiment, the special π, the test, the fruit, the symbol, the σ fruit shot No 201035159 No more precise statements are allowed under certain circumstances. It can be assumed that the actual results are significantly lower than the recorded values in individual cases. Example 2: Batch purification of a higher concentration of polythiophene solution at another higher concentration In the experiment of the thiophene solution, it was essentially the same as in Example 1, except that in contrast to Example 1, 25 ml of polybuton dissolved in tetrahydrofuran and 54 mg/kg of magnesium and 5200 mg/kg of magnesium were initially dissolved. The thiophene solution was placed outside the first vessel. Similar to Example 1, ion exchange resins (Lewatit® K2629) of different masses according to Table 2 were added to this solution and purified. Similar to Example i for analysis. --______ After purification Ni content [mg / metric jin]

Compared with T% metal / semi-# ion exchange resin mass [g] purified Mg content [mg / kg] 1 3 120 2 3.5 14 3 4 1.2 4 4.4 0.16 5 4.5 0.1 It is found that the method according to the invention can also be purified with significant A solution with a higher concentration of metal. Example 3: Batch Purification of Polythiophene Solution - Determination of Purification Time / Retention in Another Purified Polyporphin Solution Experiment, essentially the same as Example 18 201035159, except that unlike the example, 150 liters was initially dissolved in tetrahydrofuran A polythiophene solution containing 1.5% by weight/° polyporphin and 26 mg/kg of nickel and 1190 g/kg of magnesium was placed outside the first container. An ion exchange resin (Lewatit® SP112) having a mass of 13.5 g was added to this solution in each case and purified according to Table 3 at different times. The analysis was performed again similarly to Example 1. Table 3: Experimental data according to Example 3 Purification time [hour] Mg content after purification [mg/kg] Ni content after purification [亳g/kg 1 1 0.5 4.90 8.5 2 1 1.90 5.3 -3 1.5 0.90 2.1 4 2 0.50 ------ 1.1 5 4 0.20 < 0.05 6 6 0.11 < 0.05 It was found that the method according to the present invention can remove metal/half highly efficiently even after a significantly shorter time than the examples 1 and 2. metal. Based on the experimental data obtained in this batch method and the ion exchange resin loading measured by the meaning of the metal/semimetal removed per unit ion exchange resin quality, it is familiar to the skilled person that the design can be continuous in a simple manner. Purification procedure. BRIEF DESCRIPTION OF THE DRAWINGS Figure la shows the conditions when the first and second purification zones (r1vR2) are still at the full loading time t1 of the ion exchange resin (A) of the two purification zones 19 201035159. A solution comprising a semiconducting polymer and a contaminant in the form of a metal and/or semi-metal (L) is supplied to the first purification zone (Ri). The purified solution is obtained without metal and/or semi-metal (L'). Figure lb shows the conditions of the first purification zone (R) after the time when the ion exchange resin (A) is almost loaded with contaminants in the main metal and/or semimetal form and has reached a threshold value. This stream is transferred to the second reaction zone (R2) of the ion exchange resin which is still unloaded. Figure lc shows the conditions after the purification zone (3⁄4) is at the time t3 > t2 > ti of the ion exchange resin (A) completely loaded with the contaminant in the form of metal and/or semimetal (L). The stream is returned to the first reaction zone (R) of the ion-exchange resin which is again unloaded. Restart the program. [Main component symbol description]

Ri First purification zone r2 Second purification zone A Ion exchange resin L Metal and / or semi-metal L, metal and / or semi-metal 20

Claims (1)

201035159 VII. The scope of the patent application: 1. The method of human race, semiconductor polymer, characterized in that a solution containing a semiconductor polymer having 113% by weight of j is passed through - a pure immersion domain containing ion exchange difficulties, The ion exchange resin contains a sulphate group on the polystyrene-containing copolymer. 2. The method according to item i of the patent application, characterized in that the separation The copolymer of the sub-replacer resin also contains a diethylphenyl group in addition to the polystyrene group. 3. ^ According to the method of patent (4) 丨 or 2, the method is characterized in that the father replaces the fine average of the resin (four) of the particle bed of 0.01 to 2 mm. 4. According to the method of the third paragraph of the patent scope of the towel, It is characterized in that the particles have a particle size distribution of a completely single mode on the babe. 5. The method according to any one of the claims (4), wherein the particle exchange is porous. 6. A method according to the prior art, characterized in that the solution comprising a semiconducting polymer having a content of i 3 % by weight also contains a metal/semimetal content exceeding ΙΟΟΟρριη. 7. The method according to the prior application, wherein the solvent of the solution comprises a substance containing a group. 8. According to the method of claim 4 (4), the frequency is that the solvent is tetrahydrofuran or a mixture of tetrahydrofuran and toluene. 9. The method according to the first method of patent application, wherein the solution passes through a first purification zone, and the metal and/or semimetal contains 4 to straight::: region exit depreciation and characteristics In that the 201035159 solution is then passed through a second purification zone equal to the first purification zone and simultaneously exchanges or regenerates the ion exchange resin of the first purification zone. The method according to any one of the preceding claims, characterized in that it is carried out in a purification zone at a temperature of from 80 °C to 120 °C. An use of an ion exchange resin containing a sulfonic acid group on a copolymer containing a polystyrene group, which is used for purifying a solution of a metal and/or a semimetal having a semiconductor polymer content of 1 to 3% by weight. twenty two