PROCESS FOR PRODUCING A THERMOPLASTIC MATERIAL, A PROCESS OF FORMING A GRANULATE OR EXTRUDATE, THERMOPLASTIC PRODUCT AND USE OF THE THERMOPLASTIC MATERIAL

Abstract

A process for producing a thermoplastic material for use as powder or slurry for further processing such as injection molding or coating, comprising the steps of mixing a biomass containing prolamins, such as a grain source or a water insoluble fraction of a grain, having prolamins and lipids, and an organic solvent to obtain undissolved components and dissolved components comprising dissolved prolamin, lipids and other dissolved components, extracting the dissolved components into a first liquid and extracting undissolved components in a first solid under the specific conditions. separating the first solid from the first liquid, recovering the thermoplastic material from the first liquid as powder by removing organic solvent under the conditions of maintaining temperature of the prolamins below 80° C., preferably below 75° C., maintaining a dielectric constant εr between 30 and 42 at 25° C., and maintaining a pressure level at below 2 bar.

Claims

1. A process for producing a thermoplastic material for use as a powder or a slurry for further processing such as extrusion, injection molding or coating, comprising the steps: (i) mixing a biomass containing prolamins, such as a grain source or a water insoluble fraction of a grain, having prolamins and lipids, and an organic solvent to obtain undissolved components and dissolved components comprising dissolved prolamin, lipids and other dissolved components; (ii) extracting said dissolved components into a first liquid and extracting undissolved components in a first solid under the following conditions: a. maintaining temperature below 80° C., preferably below 75° C., most preferably below 70° C.; b. maintaining dielectric constant ε.sub.r (at 25° C.) between 30 and 42; c. maintain pressure level p at below 2 bar; d. performing extraction for no longer than an extraction time te (in min) = ke1 *T (in °C) + ke2* ε.sub.r (at 25° C.) + ke3*p (bar absolute), wherein ke1 is in the range between 0.04 and 1.00, ke2 is in the range between 0.08 and 2.00, and ke3 is in the range between 1.70 and 60.00; (iii) separating the first solid from the first liquid; (iv) recovering said thermoplastic material from the first liquid as powder or slurry by removing organic solvent under the following conditions: maintaining temperature of the prolamins below 80° C., preferably below 75° C., most preferably below 70° C.; maintaining a dielectric constant ε.sub.r (at 25° C.) between 30 and 42; maintaining a pressure level at below 2 bar; and performing recovering for no longer than a recovering time t (in min) = kr1*T (in °C) + kr2* εr (at 25° C.) + kr3*p (bar absolute) where kr1 is in the range between 0.0004 and 12.0000, kr2 is in the range between 0.0008 and 7.0000, and kr3 is in the range between 0.0167and 80000.0000.

2. The process according to claim 1, comprising the step of filtering, by membrane filtration, the first liquid to at least partly remove said other dissolved components other than prolamin and lipids from the first liquid, said filtering being performed under the following conditions maintaining temperature below 80° C., preferably below 75° C., most preferably below 70° C., even more preferably below °40C; maintaining dielectric constant between εr(at 25° C.) between 30 and 42; maintaining a pressure level below 7 bar.

3. The process according to claim 2, wherein the filtration is a two-stage filtration, wherein the first filter stage is a filtration with a first membrane with a size comprises between 4 and 10 kg/mol and the second filter stage is a filtration with a second membrane with a size comprised between 0.2 and 1.0 kg/mol.

4. The process according to claim 1, wherein the prolamins have naturally grown prolamin structures and distributions and the lipids have naturally grown lipid content and distribution.

5. The process according to claim 1, wherein the first liquid is treated to increase viscosity.

6. The process according to claim 1, wherein the first liquid comprises either a) ethanol in an amount of 50 to 90%, preferably 55 to 85%, more preferably 60 to 80%, most preferably 65 to 75% (v/v); or b) isopropanol in an amount of 40 to 80%, preferably 45 to 75%, more preferably 50 to 70%, most preferably 55 to 65% (v/v).

7. The process according to claim 1, wherein the content of lipids with respect to the dry mass is maintained throughout the process to be above 4 percent in weight, preferably between 4 and 23%.

8. The process according to claim 7, in which the content of lipid with respect to the dry mass in the biomass containing prolamin such as corn gluten meal is between 2 and 7% in the corn gluten, and between 10 and 20% in the first liquid.

9. The process according to claim 1 wherein ratios among the lipids/fatty acids are maintained throughout the entire process at the following levels in wt.-% of total lipids: free fatty acids / monoglycerides / diglycerides / triglycerides 91+/-6 / 3+/-2 / 5+/-3 / 1+/-1.

10. The process according to claim 1, wherein a protein content being defined as the ratio between the mass of the protein and the total dry mass is kept at a level below 95 wt.% throughout the entire process.

11. The process according to claim 1, wherein a ratio between alpha helix and beta-sheet in the secondary structure is maintained throughout the entire process, preferably at least at the ratio between alpha helix and beta-sheet in the secondary structure of the corn gluten meal, most preferably at a level of at least 1.6.

12. The process according to claim 1, further comprising adding additives.

13. A process of forming a granulate or extrudate comprising the steps of providing a thermoplastic material by a process of claim 1, wherein the coating is obtained by at least one of wet casting on paper by roll-to-roll coating or slot die coating or extrusion on a support such as paper and/or a rigid mold is obtained by injection molding of the thermoplastic material using the obtained powder and/or a granulate/extrudate obtained by way of extruding said powder.

14. The process of claim 13, comprising dissolving the powder and/or adding additives to the powder, slurry, and/or dissolved powder.

15. A thermoplastic product obtained from biomass containing prolamins such as from a grain source or a water insoluble fraction of a grain having prolamins and lipids, in particular resulting from a process according to claim 1, yielding: at a melt volume rate of between 1 and 200 cm3/10 min, at 5 kg, at a temperature between 100 and 150° C.

16. Use of a thermoplastic product obtained from biomass containing prolamins such as from a grain source or a water insoluble fraction of a grain having prolamins and lipids, in particular product resulting from a process according to claim 1 as an injection molded product or as a coating.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0084] In the drawings:

[0085] FIG. 1 illustrates a process scheme of an integrated process according to an embodiment of the present invention.

[0086] FIG. 2 illustrates a process scheme of an integrated process according to another embodiment of the present invention.

[0087] FIG. 3 illustrates a process scheme of an integrated process according to another embodiment of the present invention

[0088] FIG. 4 illustrates a curve of the dielectric constant (at 25° C.) as a function of the concentration of ethanol.

[0089] FIG. 5 is a table of characteristics for different illustrative and comparative materials.

[0090] FIGS. 6A, 6B, 6C, 7A, 7B, 8A, 8B, 9A, 9B, 9C, 10A, 10B, 11A, 11B, 12A, 12B and 13 show images of the materials produced.

DETAILED DESCRIPTION OF THE INVENTION

[0091] The process according to the present invention produces a thermoplastic material with good physicochemical and mechanical properties from a corn gluten source. A thermoplastic material as understood herein means a material that comprises all constituents required for being formed into a rigid mold or a coating. In some embodiments, all constituents of the thermoplastic material stem from the corn gluten source and no external constituents are added. In some embodiments, the thermoplastic material additionally comprises external constituents.

[0092] The term “flexible thermoplastic material” denotes a thermoplastic material that can be used as a flexible film or coating. In contrast, the term “rigid thermoplastic material” refers to a thermoplastic material, which can be formed into a rigid thermoplastic article.

[0093] The thermoplastic materials are a class of materials that can be softened and melted by the application of heat and can be processed in the heat-softened state, e.g., by extrusion and injection molding. The thermoplastic materials can be remolded and recycled without negatively affecting the thermoplastic materials physical properties.

[0094] The organic solvent may comprise a mixture of two or more organic solvents, or a mixture of at least one organic solvent and an aqueous solvent. The amount and type of organic solvent(s), and optionally the amount and type of the aqueous solvent, are selected so that the resulting composition (i.e., the first liquid) is capable to serve as an extracting solvent for certain components of the corn gluten source (herein referred to as the solvent-soluble components).

[0095] The primary aim of the extraction of the solvent-soluble components is to obtain a liquid phase (herein referred to as the first liquid), which is enriched in thermoplastic forming components, in particular in corn gluten proteins and lipids, and depleted in carbohydrates, lignin and minerals.

[0096] Accordingly, the solvent is preferably selected based on its capability of dissolving biomass having prolamin in particular prolamins and corn gluten lipids, in particular corn gluten fatty acids. It is further preferred that the solvent does not dissolve fibers to a substantial extent.

[0097] In preferred embodiments, the organic solvent is selected from the group consisting of aprotic polar organic solvents, protic organic solvents and mixtures thereof. Preferably, the organic solvent is selected from the group consisting of alcohol, ketones, and mixtures thereof. More preferably, the organic solvent is selected from the group consisting of monovalent alcohols containing 1 to 6, 1 to 5, 1 to 4, or 1 to 3 carbon atoms, and mixtures thereof. Most preferably, the organic solvent is selected from the group consisting of ethanol, isopropanol, and mixtures thereof.

[0098] According to one embodiment, the solvent may be an aqueous phase comprising ethanol in an amount of 50 to 90%, preferably 55 to 85%, more preferably 60 to 80%, most preferably 65 to 75% (v/v). Thereby, it is ensured that the ethanol content is close to the optimum, which has been determined to be 70% (v/v).

[0099] According to another embodiment, the solvent may be an aqueous phase comprising isopropanol in an amount of 40 to 80%, preferably 45 to 75%, more preferably 50 to 70%, most preferably 55 to 65% (v/v). The optimal isopropanol content has been determined to be 60% (v/v). The preferred ranges have thus been selected for being close to the optimal isopropanol content.

[0100] With respect to other solvents or solvent combinations that are useful in the context of the present invention, one may consider solvents having a similar logP value as ethanol, isopropanol, or as the resulting solvent comprising ethanol or isopropanol in the above amount. Moreover, one may take into account the solvents’ tendency of dissolving desired components, namely prolamin, while not dissolving not desired components, as explained above.

[0101] As mentioned above, the solvent-soluble components of the biomass comprising prolamins such as corn gluten source are extracted from the first solid into the first liquid. The term “biomass” should be understood as a biomass comprising at least 15 wt.% of carbohydrates or at most 50 wt. % of prolamins or at most 70 wt.% of proteins. As such the zein is not to be considered as biomass in the context of the present invention. The term “solvent-soluble components” denotes one or more components, which are soluble in the first liquid under the conditions applied during the extraction. The components comprise corn gluten proteins and corn gluten lipids, preferably fatty acids. By extracting both corn gluten proteins and lipids, a thermoplastic material can be produced without having to add external fatty acids or another plasticizer in order to be processed via conventional thermoplastic related conversion techniques.

[0102] The extraction may be carried out at ambient temperature, e.g., around 20° C. In preferred embodiments of the present invention, the extraction involves heating and/or mixing. Thereby, the process step can be accelerated, and its yield increased. For example, the extraction may be carried out at a temperature of at least 25° C., preferably at least 30° C., more preferably at least 40° C., more preferably at least 50° C., most preferably at least 55° C. In terms of power consumption, it may be advisable to limit the maximum temperature. Accordingly, the extraction is preferably carried out at a temperature of at most 80° C., preferably at most 75° C., more preferably at most 70° C., more preferably at most 65° C., most preferably at most 60° C.

[0103] The duration needed for extraction is not particularly limited and may generally range between 1 or several minutes, e.g., 5 minutes, and 24 hours.

[0104] In one embodiment, the duration needed for extraction is between 10 min and 3 hours.

[0105] The first solid and the first liquid are separated. This can be achieved by removing the first solid (including solvent-non-soluble components of the biomass containing prolamins, e.g., of the corn gluten source) from the first liquid by solid-liquid separation, preferably by centrifugation, filtration, decantation, sedimentation, or a combination thereof.

[0106] The dielectric constant εr is maintained between 30 and 42 at 25° C. by maintaining the concentration of the organic solvent between 40 and 90 vol.%, preferably between 70 and 90 vol.%.

[0107] For example, the organic solvent can be isopropanol at a concentration of 40 to 85 vol.%. In another example, the concentration of isopropanol is 60 to 85 vol%. In a further example, the organic solvent is ethanol at a concentration of 60 to 90 vol.%., preferably 70 to 90 vol.%.

[0108] FIG. 4 illustrates a curve of the dielectric constant (at 25° C.) as a function of the concentration of ethanol as used in the present disclosure. A linear regression of the curve can be seen on FIG. 4.

[0109] Most surprisingly the applicant has found that adjusting the dielectric characteristics of the solvent allows to arrive at suitable thermoplastic material having high suitability for further processing such as injection molding. Indeed, the applicant has found that best further processing is available if a major part of the prolamins, substantially all the prolamins are kept in the naturally grown structure and interaction with the originally present lipids, possibly with optional further additives. This is in contrast to the teachings in the prior art during manufacturing of commercial Zein, where in at least one step water is added to the dissolved Zein on purpose. The prior art discloses adding water in the process for zein recovery. Therefore, the prior art encourages the person skilled in the art to precipitate zein in water, therefore, changing the prolamins naturally grown structure. The prior art also discloses that water is a preferred compound and should be added as an additive to reach advantageous properties. Hence the prior art generally suggests changing the dielectric constant during the manufacturing process. It is therefore surprising that a process for producing a thermoplastic material for multiple possible use for injection molding, as a film or as a flexible or non-flexible coating results in clearly different products as to processability by respecting the parameters as claimed and in particular by maintaining the dielectric constant unchanged.

[0110] Accordingly, in the process of the present invention, the dielectric properties of the first liquid are adjusted to keep fatty acids in the first liquid phase. Hence, the desired dissolved components will remain in the liquid phase, whereupon one can optionally perform filtration. This approach is in full contrast to the known processes, always aiming at reducing oil content and to recover all of the prolamin.

[0111] Indeed, the applicant has found that the characteristics of prolamin having the initial lipids and in particular fatty acids shows much better properties as compared to prolamin from which fatty acids have been extracted. This has proven even more true if the structure of the prolamin has not been altered, such as in zein.

[0112] The Applicant has also found that the characteristics of prolamin having a part of initial lipids and in particular a part of the fatty acids shows good properties.

[0113] The various features and embodiments described in the context of the methods of the invention shall be understood to define corresponding features and embodiments of the apparatus of the invention, and vice versa.

[0114] Further embodiments of the present invention are described with reference to the process scheme shown in FIG. 1 to FIG. 3.

[0115] FIG. 1 illustrates a process scheme of an integrated process integrating a process according to an embodiment of the present invention.

[0116] In a first step S1: a prolamin containing biomass is mixed with a solvent. The solvent has a dielectric constant between 30 and 42 (at 25° C.), the mixing is performed in the ratio 1:4 to 1:10 substrate/solvent (w/w), for a time of 10 to 180 min.

[0117] Then, in step 2, the solids are separated from the liquid phase, thereby obtaining a first liquid and a first solid. The first liquid may be separated from the solids (herein referred to as the first solid) by centrifugation. The solids may be removed from the process and used as feedstuff for animals or the like. The first liquid is further processed.

[0118] In the third step, the first liquid is dried, thereby obtaining a powder.

[0119] The powder is subsequently to the inventive process mixed (step 4) with additives in an extruder to obtain a granulate. The granulates can be processed (step 5) in an injection molding machine or in a paper extrusion to obtain a rigid mold or coated paper.

[0120] FIG. 2 illustrates a process scheme of an integrated process according to an embodiment of the present invention.

[0121] In the first step, a prolamin containing biomass is mixed with a solvent. The solvent has a dielectric constant of 30 to 42 (at 25° C.). The mixing is done in the ratio 1:4 to 1:10 substrate/solvent (w/w), for a time of 10 to 180 min. The solids are then separated from the liquid phase, thereby obtaining a first liquid and a first solid (step 2).

[0122] An additional step of filtration (Step 3) is performed. The first liquid is concentrated to increase the dry matter content and mixed with additives to obtain a second liquid. In the next step 4, the second liquid is dried, thereby obtaining a powder.

[0123] Finally, the powder can be processed (step 5) in an extruder to obtain a granulate, and the granulates are processed (step 6) in an injection molding machine or in a paper extrusion to obtain a rigid mold or coated paper

[0124] FIG. 3 illustrates a process scheme of an integrated process integrating a process according to another embodiment of the present invention.

[0125] In the first step 1, a prolamin containing biomass is mixed with a solvent. The solvent has a dielectric constant of 30 to 42 (at 25° C.). The mixing is done in the ratio 1:4 to 1:10 substrate/solvent (w/w), for a time of 10 to 180 min. The solids are then separated from the liquid phase, thereby obtaining a first liquid and a first solid (step 2).

[0126] The first liquid is then concentrated to increase the dry matter content and mixed with additives. In the next step 4, the resulting mixture is dried, thereby obtaining a powder.

[0127] The drying is conducted in a casting machine at a temperature between 50° C. and 100° C. for a time of 10 min to 5 hours.

[0128] Then, in a step subsequent to the inventive process in step 5, the powder is mixed with a solvent having a dielectric constant between 30 and 42 at 25° C., to obtain a third liquid.

[0129] Finally, in step 6, the step of coating the third liquid on a paper surface is performed, to obtain a coated paper. This can be done using for example roll-to-roll coating or slot die coating.

[0130] Although, the quality of the obtained thermoplastic material is hardly explainable the applicants assume that maintaining the specific process parameters is avoiding that the apparent interaction existing between prolamin, and lipids be impaired. Most surprisingly it has proven that avoiding denaturation and trying not to alter the lipid concentration and distribution results in bio thermoplastic materials having characteristics not obtainable so far and this even in an industrial scale.

[0131] In the following, the invention is explained in more detail by means of selected examples.

[0132] Example 1: Corn gluten meal was obtained from a starch production plant. The corn gluten meal was then mixed with an ethanol-mixture with a dielectric constant of 35. The mixture was heated to 50° C. and then stirred at 50° C. for two hours. Afterwards, solids were removed without cooling by centrifugation for 5 min at 5000 × g. The recovered supernatant was filtered in a membrane filtration at 4 kDa and 7 bar at room temperature until a viscous liquid as the first retentate was formed. The permeate was filtered through a 200 Da membrane until a viscous liquid as the second retentate was formed. The first retentate and the second retentate were combined and mixed with 20 wt.-% glycerol, then dried at room temperature, then milled to a powder and sieved to < 2 mm. Subsequently to the inventive process the powder is then extruded to granulates at 130° C. The granulates showed good thermoplastic properties, by having a melt flow index of 45 g / 10 min (5 kg).

[0133] Example 2: The process of Example 1 where the powder was mixed with the 2-fold amount of ethanol-mixture (by weight) and with 20 wt.-% polyols. The obtained solution was stirred for 10 min in a speed mixer at room temperature and then coated on a paper and dried at room temperature to form a 20 .Math.m paper coating. The coating showed a good flexibility (8% elongation at break), high fat barrier (KIT 14) and high seal strength (4.3 N/15 cm).

[0134] Example 3: The process of Example 1 where the dielectric constant of the solvent during the extraction was changed to 38, which resulted in the same product quality.

[0135] Example 4: The process of Example 1 where the extraction temperature was changed to 65° C., which resulted in the same product quality.

[0136] Example 5: The process of Example 1 where the recovered supernatant was dried in a spray dryer at 80° C., which resulted in the same product quality.

[0137] Example 6: The process of Example 1 where the granulate was processed in an injection molding machine, which resulted in rigid forms with good mechanical properties (tensile strength 40-50 MPa).

[0138] Example 7: The process of Example 1 where the dielectric constant during the extraction was changed to 50, where the resulting product showed no thermoplastic properties and could not be extruded.

[0139] Example 8: The process of Example 1 where the dielectric constant during the extraction was changed to 60, where the resulting product showed no thermoplastic properties and could not be extruded.

[0140] Example 9: The process of Example 1 where the drying temperature was changed to 110° C., where the resulting product showed no thermoplastic properties and could not be extruded.

[0141] Further examples are provided below. The process of producing the materials of examples 10 to 18 below does not necessarily comprise adding additives at a fixed concentration to facilitate the process.

[0142] The MFI is a measure of the ease of flow of the melt of a thermoplastic material. The MFI is defined as the weight of the material in grams flowing in 10 min through a die of specific diameter and length by a pressure applied by a given weight at a given temperature. The melt flow index test procedure comprises placing the material to be tested in a small tank with a thin tube at the end of the tank, with a diameter of 2.095 mm and a length of 8 mm. The material is heated to a certain temperature and then the upper end of the material is pushed downward by a piston through pressure extrusion. The MFI of raw material is measured in 10 minutes by the weight of the extruded material corresponding to the melt flow index of the material.

[0143] An MFI value of 25 g / 10 min means that 25 g of material is extruded in 10 minutes. The MFI of common plastics ranges from 1 to 45.

[0144] In one example, the thermoplastic material X is produced according to the present invention from a biomass. The recovered supernatant is directly applied for recovery of thermoplastic material The produced thermoplastic material X comprises a protein content of 74 to 78%.

[0145] In another example, the thermoplastic material Y is produced according to the present invention from a pre-treated biomass. The recovered supernatant is directly applied for recovery of thermoplastic material. The produced material Y comprises a protein content of 78 to 95%.

[0146] A comparison has further been conducted between the thermoplastic material X, the thermoplastic material Y, both produced according to the present invention and a commercial zein being sold as purified zein. Additives were added to the thermoplastic material X, the thermoplastic material Y and the commercial zein to determine if the increase of the additive amount is followed by an improvement of the thermoplastic behavior of the materials and to compare the processability of the thermoplastic material X, the thermoplastic material Y and the commercial zein. The commercial zein is not a biomass as defined in the present invention. The composition of the thermoplastic material X, the thermoplastic material Y and the commercial zein can be found in FIG. 5. The concentrations of additives are chosen with the intent of maintaining the relative amount of the recovered thermoplastic material as high as possible for economic reasons. The concentration of additives in the examples below enables to obtain material with thermoplastic properties that is minimally processable. NV stands for no values. In the following examples for illustration purpose only, the additives could be among others carboxylic acid (Examples 10, 11, 12, 15 and 16 with carboxylic acid 1 as additive; Examples 13 and 14 with carboxylic acid 2 as additive).

[0147] Example 10: Commercial zein + 15% (w/w) additives (Comparative Example)

[0148] The produced material shows a substantial inflating and hardening behavior. The substantial inflating and the hardening behavior occur before any significant melting process, making the measurement of an MFI value impossible to obtain. The produced material appears sticky, making the cutting of the produced pieces of material difficult. The produced material needed to be forcefully pulled out of the nozzle of the extruder used and shows a fibrillar appearance, as can be seen on FIGS. 6A, 6B and 6C. This can be attributed to the beginning of a decomposition process, which impacts the re-meltability of zein, invalidating the possibility of items produced with commercial zein to be remelted and recycled.

[0149] The results indicate no suitability of commercial zein for conventional thermoplastic related conversion techniques when mixed with additives at a concentration of 15% (w/w).

[0150] Example 11: thermoplastic material X + 15% (w/w) additives (Illustrative Example)

[0151] The produced material is extruded with ease and a series of extrudate segments with uniform length can be obtained, as can be seen on FIGS. 7A and 7B. This proves the occurrence of a melting process during the measurement and thus that the process enables the obtention of a thermoplastic material. The produced material also shows no sign of decomposition, suggesting the ability of the produced material of Example 11 to be remolten and recycled.

[0152] Example 12: thermoplastic material Y + 15% (w/w) additives (Illustrative Example)

[0153] The material is produced from a pre-treated biomass containing prolamins and lipids and is extruded with ease and a series of extrudate segments with uniform length can be obtained, as can be seen on FIGS. 8A and 8B. This proves the occurrence of a melting process during the measurement and thus that the process enables the obtention of a thermoplastic material. The produced material also shows no sign of decomposition, suggesting the ability of the produced material of Example 12 to be remolten and recycled. The added additive in example 12 can be seen as a plasticizer or a lubricant in the process.

[0154] The results indicate the suitability of the produced material of Example 12 for conventional thermoplastic related conversion techniques when mixed with additives at a concentration of 15% (w/w).

[0155] Example 13: Commercial zein + 5% (w/w) additives (Comparative Example)

[0156] It was possible to forcefully push the produced material out of the nozzle, however the filaments obtained were not homogeneous and extremely brittle, making the measurement of an MFI value impossible to obtain. Moreover, the produced material is inflated during the measurement. Although it is possible to force a filament out of the nozzle, the produced material of Example 13 is so brittle that it is possible to crumble the produced material by touching, as can be seen on FIGS. 9A, 9B and 9C.

[0157] The results indicate no suitability of the commercial zein for conventional thermoplastic related conversion techniques when mixed with additives at a concentration of 5% (w/w).

[0158] Example 14: thermoplastic material X + 5% (w/w) additives (Illustrative Example)

[0159] The produced material is extruded with ease and a series of extrudate segments with uniform length can be obtained, as can be seen on FIGS. 10A and 10B. This proves the occurrence of a melting process during the measurement and thus that the process enables the obtention of a thermoplastic material. The produced material also shows no sign of decomposition, suggesting the ability of the produced material of Example 14 to be remolten and recycled.

[0160] The results indicate the suitability of the produced material of Example 14 for conventional thermoplastic related conversion techniques when mixed with additives at a concentration of 20% (w/w).

[0161] Example 15: Commercial zein + 20% (w/w) additives (Comparative Example)

[0162] It was not possible to push the sample out of the nozzle, as can be seen on FIGS. 11A and 11B. Only a minimal amount was observable from the other end of the measuring tube simply due to the complete filling of such tube, making the measurement of an MFI value impossible to obtain. Moreover, the produced material results in extremely sticky. Similarly, to Example 10, also this one needed to be forcefully pulled out of the nozzle and showed a fibrillar appearance.

[0163] The results indicate no suitability of the commercial zein for conventional thermoplastic related conversion techniques when mixed with additives at a concentration of 20% (w/w).

[0164] Example 16: thermoplastic material Y + 20% (w/w) additives (Illustrative Example)

[0165] The produced material is extruded with ease and a series of extrudate segments with uniform length can be obtained, as can be seen on FIGS. 12A and 12B. This proves the occurrence of a melting process during the measurement and thus that the process enables the obtention of a thermoplastic material. The produced material also shows no sign of decomposition, suggesting the ability of the produced material of Example 16 to be remolten and recycled.

[0166] The results indicate the suitability of the produced material of Example 16 for conventional thermoplastic related conversion techniques when mixed with additives at a concentration of 20% (w/w).

[0167] Example 17: thermoplastic material X + 0% (w/w) additive

[0168] The thermoplastic material X was extrudable without the addition of an additive. FIG. 13 shows an extrudate that is soft. FIG. 13 further shows that extrusion is possible and that the process can be processed smoothly. The sample was extruded with ease and a series of extrudate segments with uniform length could be obtained. This proves the occurrence of a melting process during the measurement and thus of thermoplastic behavior. The samples of Example 17 also show no sign of decomposition, suggesting their ability to be remolten and recycled.

[0169] The results indicate the suitability of example 17 for any thermoplastic related conversions with no additive.

[0170] Example 18: Commercial zein X + 0% (w/w) additive

[0171] In contrast, zein without the addition of plasticizer does not show any extrudability.

[0172] The value of MFI and statement of extrudability for each example can be found in FIG. 5.

[0173] As can be seen from the above results of the melt flow index (MFI) and the figures obtained with different levels and types of additives, products obtained by the process of the present disclosure need significantly lower amounts of plasticizers in contrast to the commercially available zein. Indeed, commercial zein is produced in a process where the first liquid phase is poured into water, changing the dielectric constant to >42, typically in the range of 50 to 75. That causes re-structuring of the proteins with subsequent precipitation, which is unfavorable for the use as thermoplastic product.

[0174] A comparison of the examples shows that the process according to an embodiment of the present invention significantly improves the thermoplastic characteristics and the suitability for further processing such as by injection molding as compared to a state-of-the-art process.

[0175] The foregoing description of the preferred embodiment of the invention has been presented for purposes of illustration and description. It is not intended to be exhaustive or to limit the invention to the precise form disclosed, and modifications and variations are possible in light of the above teachings or may be acquired from practice of the invention. The embodiment was chosen and described to explain the principles of the invention and its practical application to enable one skilled in the art to utilize the invention in various embodiments as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims appended hereto and their equivalents. The entirety of each of the aforementioned documents is incorporated by reference herein.