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Brevet US4076846 - Protein-starch binary molding composition and shaped articles obtained therefor - Google�BrevetsRecherche Images Maps Play YouTube Actualit�s Gmail Drive Plus »Connexion BrevetsAn edible, water-soluble, thermoplastic molding composition comprising a starch material, a neutral inorganic alkali salt of protein material, water, an edible plasticizer, an edible lubricant, and other additives. This composition shows excellent moldability and processability when subjected to various...http://www.google.fr/patents/US4076846?utm_source=gb-gplus-shareBrevet US4076846 - Protein-starch binary molding composition and shaped articles obtained therefor Recherche avanc�e dans les brevets Num�ro de publicationUS4076846 AType de publicationOctroi Num�ro de demandeUS 05/631,405 Date de publication28 f�vr. 1978 Date de d�p�t12 nov. 1975 Date de priorit�22 nov. 1974 Num�ro de publication05631405, 631405, US 4076846 A, US 4076846A, US-A-4076846, US4076846 A, US4076846A InventeursRyuzo Nakatsuka, Setsuo Suzuki, Shinichi Tanimoto, Eiji Funatsu Cessionnaire d'origineSumitomo Bakelite Company LimitedExporter la citationBiBTeX, EndNote, RefManCitations de brevets (3), R�f�renc� par (187), Classifications (50) Liens externes: USPTO, Cession USPTO, EspacenetProtein-starch binary molding composition and shaped articles obtained therefor
US 4076846 A R�sum�
An edible, water-soluble, thermoplastic molding composition comprising a starch material, a neutral inorganic alkali salt of protein material, water, an edible plasticizer, an edible lubricant, and other additives. This composition shows excellent moldability and processability when subjected to various constomery dry processes for molding and processing customary plastics, such as compression molding, transfer molding, extrusion molding, blow molding, inflation molding, injection molding, vacuum forming, pressure forming, heat sealing, etc. Transparent or translucent shaped articles obtained from the above composition have unique properties such as gas impermeability, solubility in water, edibility, biodegradability, etc., and may be utilized with favorable results in various fields such as food industry, feedstuff industry, agriculture, fisheries, etc. The shaped articles, if necessary, can be allowed to have any balance between its water resistance and its water-solubility by ultraviolet irradiation or by the incorporation of a protein-coagulating agent.
1. A water-soluble and edible thermoplastic molding composition comprising:a starch material; a protein material; water; an organic, low-molecular-weight plasticizer; and a lubricant; said starch material being at least one edible, natural, unmodified starch; said protein material being at least one edible protein salt selected from the group consisting of sodium, potassium and calcium salts of edible, natural protein concentrates; said organic low-molecular-weight plasticizer being at least one edible, polyhydric alcohol selected from the group consisting of glycerol, ethylene glycol, diethylene glycol, sorbitol, sorbitan, mannitol, maltitol, hydrogenated starch syrup, and sucrose; and said lubricant being at least one lubricant selected from the group consisting of mono-, di and tri-esters of said edible, polyhydric alcohols with edible higher fatty acids having at least 10 carbon atoms, phosphoric acid derivatives of said esters and lecithin; said starch containing at least 50% by weight of amylose; the weight ratio of said starch to said protein salt being 30/70 to 70/30; the water content of the composition being 10 to 40% by weight based on the total weight of the composition; and the amount of said organic, low-molecular-weight plasticizer and that of said lubricant being, respectively, 20 to 60 parts by weight and 1 to 11 parts by weight per 100 parts by weight, in total, of said starch and said protein salt. 2. A molding composition according to claim 1, wherein the starch is one which has been previously transformed into α-type.
8. A method for manufacturing a water-soluble and edible thermoplastic molding composition in the granular form, which comprises:heating and mixing at 50� C or more a blend of (A) at least one edible natural unmodified starch, (B) at least one edible natural protein concentrate, (C) an aqueous dispersion of at least one inorganic alkali selected from the group consisting of sodium, potassium and calcium hydroxides, carbonates and bicarbonates, to form a salt of the protein, (D) at least one edible organic low-molecular-weight plasticizer selected from the group consisting of glycerol, ethylene glycol, sorbitol, sorbitan, mannitol, maltitol, hydrogenated starch syrup, and sucrose, and (E) at least one lubricant selected from the group consisting of mono-, di- and tri-esters of the edible polyhydric alcohols set forth in (D) with edible higher fatty acids having at least 10 carbon atoms, phosphoric acid derivatives of said esters and lecithin; said starch material containing at least 50% by weight of amylose; the weight ratio of said starch material to said protein salt being 30/70 to 70/30; the amount of said organic low-molecular-weight plasticizer and that of said lubricant being, respectively, 20 to 60 parts by weight and 1 to 11 parts by weight per 100 parts by weight, in total, of said starch material and said protein salt; and the amount of said aqueous dispersion of at least one inorganic alkali being sufficient enough to substantially neutralize said protein; while gradually adding further water and thereafter granulating the blend and finally adjusting the water content in the composition to 10 to 40% by weight. 9. A method according to claim 8, wherein the edible natural protein concentrate is casein and the aqueous dispersion of inorganic alkali is an aqueous sodium hydroxide solution.
10. A method for manufacturing a water-soluble and edible thermoplastic extrusion-molded article, which comprises:heating, mixing and granulating a blend of a starch material, a protein material, water, an organic low-molecular-weight plasticizer and a lubricant to form a thermoplastic molding material; introducing the molding material into the heated barrel of an extruder; mixing the composition under pressure in the extruder, and then extruding the mixed composition through a die; and finally adjusting the water content in the resulting molded article to 5 to 30% by weight; said protein material being at least one edible protein salt selected from the group consisting of edible neutral salts of sodium, potassium and calcium with edible natural protein concentrates; said organic low-molecular-weight plasticizer being at least one edible polyhydride alcohol selected from the group consisting of glycerol, ethylene glycol, diethylene glycol, sorbitol, sorbitan, mannitol, maltitol, hydrogenated starch syrup and sucrose; said lubricant being at least one member selected from the group consisting of mono-, di- and tri-esters of said edible polyhydric alcohols with edible higher fatty acids having at least 10 carbon atoms, phosphoric acid derivatives of said esters and lecithin; said starch material being at least one edible natural unmodified starch, and containing at least 50% by weight of amylose; the weight ratio of said starch material to said protein salt being 30/70 to 70/30; the water content in the composition being 10 to 40% by weight; and the amount of said organic low-molecular-weight polasticizer and that of said lubricant being, respectively, 20 to 60 parts by weight and 1 to 11 parts by weight per 100 parts by weight, in total, of said starch material and said protein salt; said heating and mixing being effected at a temperature of 40� C to 160� C, said extruder having a L/D of 20 to 30 and a screw compression ratio of 1.5 to 4.5, the extrusion conditions being such that the barrel under the hopper is cooled with water, the barrel temperature is 90-200� C, the die temperature is 70-120� C, and the barrel internal pressure is 10-150 kg/cm2. 11. A method according to claim 10, wherein the edible protein salt is a mixture of (A) at least one edible natural protein concentrate and (B) an aqueous dispersion of at least one inorganic alkali selected from the group consisting of sodium, potassium and calcium hydroxides, carbonates and bicarbonates in an amount sufficient to substantially neutralize the protein concentrate.
16. A method for manufacturing a water-soluble edible thermoplastic injection-molded article, which comprises:heating, mixing and granulating a blend of a starch material, a protein material, water, an organic low-molecular-weight plasticizer, and lubricant to form a thermoplastic molding composition in granular form; introducing the molding composition into the heated barrel of an injection machine; injecting the composition under pressure into a mold maintained at a temperature slightly lower than that of said barrel to fill the mold cavity; and then adjusting the water content in the resulting molded article to 5 to 30% by weight; said starch material being at least one edible natural unmodified starch; said protein material being at least one edible protein salt selected from the group consisting of edible neutral salts of sodium, potassium, and calcium with edible natural protein concentrates; said organic low-molecular-weight plasticizer being at last one edible polyhydric alcohol selected from the group consisting of glycerol, ethylene glycol, diethylene glycol, sorbitol, sorbitan, mannitol, maltitol, hydrogenated starch syrup, and sucrose; said lubricant being at least one member selected from the group consisting of mono-, di- and tri-esters of said edible polyhydric alcohols with edible higher fatty acids having at least 10 carbon atoms, phosphoric acid derivatives of said esters and lecithin; said starch material in the molding composition containing at least 50% by weight of amylose; the weight ratio of said starch material to said protein salt being 30/70 to 70/30; the water content in the molding composition being 10 to 40% by weight; the amount of said organic low-molecular-weight plasticizer and that of said lubricant being, respectively, 20 to 60 parts by weight and 1 to 11 parts by weight per 100 parts by weight, in total, of said starch material and said protein salt; said heating and mixing being effected at 40�-160� C the injection-molding conditions being such that the barrel temperature is 100-200� C, the mold temperature is up to 80� C, and the injection pressure is 10 kg/cm2 or more. 17. A method according to claim 16, wherein the edible protein salt is sodium caseinate.
There is another proposal to improve the above-said method by mixing untreated type and amylose with water and a low-molecular-weight organic plasticizer having a vapor pressure of 100 mmHg or less at 100� C., such as glycerol, ethylene glycol, propylene glycol, dimethylformaldehyde, or the like, subjecting the mixture to a high shearing stress, and extruding the resulting homogeneous fluid maintained at a high temperature through a die. The addition of a low-molecular-weight plasticizer alone has the following fatal disadvantages: (1) Because of its limited compatibility with starch, if a low-molecular-weight plasticizer is added in an amount exceeding 40 parts by weight per 100 parts by weight of starch, there is obtained on extrusion at elevated temperatures a soft, fragile, and non-sticky extrudate which cannot withstand the tension exerted by a takeoff winder, rendering the film formation under tension quite difficult. (2) Being hard and brittle on drying, as is well known, starch products require a large amount of plasticizer, the excess of which tends to cause so-called bleeding phenomenon, particularly under an atmosphere of high humidity, thus spoiling the product. (3) From the standpoint of edibility, there are only the limited number of suitable low-molecular-weight plasticizers compatible with starch, including water, glycerol, sorbitol, manitol and maltitol in all, which, however, have a reduced plasticizing action at low humidities and a tendency to bleed at high humidities. (4) Addition of a combination of water and a water-soluble polymer such as polyvinyl alcohol, in accordance with a proposal, does not sufficiently improve either the bleeding phenomenon or deficient extensibility, elongation, and strength at elevated temperatures; such a combination, in addition, is out of the question from the standpoint of environment preservation and edibility.
The present composition is manufactured by uniformly mixing the components. The mixing is carried out in various ways such as, for example, simple blending at room temperature by use of an agitated blender and milling while heating at 40� to 50� C. or at higher temperatures by use of a heated milling equipment such as Henschel mixer, roll mill, pressure kneader, or extruder. The milled mass is granulated or ground after cooling to obtain a granulated or powdered composition which is preferred to a simply blended molding composition, because the former composition is more uniformly feedable through a hopper to an extruder or injection machine, can be remilled under milder conditions in an extruder or injection machine, and can yield more uniform articles by extrusion, injection molding, etc.
A molded article of predetermined shape is obtained by feeding the present molding composition through a hopper to an extruder or injection machine maintained at 100� C. or higher temperatures, milling the composition therein with heating, and injecting the milled and melt composition into a mold maintained 90� C. or lower temperatures or extruding through a die maintained at 100� C. or lower temperatures. Since the binary blend of the inorganic alkali salt of protein material and the starch material used in the present composition exhibits a favorable melt fluidity and extensibility inspite of reduced water content, the present composition is advantageously extruded through the die or injected into the mold cavity. The extruded film may be further subjected to calendering treatment to increase the commercial value of the product.
Barrel: Water-cooled at feed point. Barrel temperature, 90� - 200� C., preferably 100� - 170� C. Internal pressure, 10 - 150 kg/cm2 Die: 70� - 120� C., preferably 70� - 100� C.
The present composition is injected under the following conditions: temperature in the barrel should be in the range from 100� to 200� C., because below 100� C. the molding compositions have no sufficient melt fluidity for molding, whereas above 200� C. they discolour markedly due to decomposition of amylose; injection pressure should be 10 kg/cm2 or higher, because below this limit gas bubbles are formed within the molded article, leading to defective products; mold temperature should be 90� C. or lower, because above 90� C. the molded article becomes so soft that the molded article is not regularly discharged by the knockout pin and continuous molding operation becomes difficult. When the compositions are injected under proper conditions outlines above, there is produced with a high efficiency transparent or translucent molded articles which have favorable moisture resistance. Thus, according to this invention, there is provided a commercially practicable novel technique for the continuous production of molded articles or predetermined shape from a binary blend of the inorganic alkali salt of protein material and the starch material.
______________________________________               PartsHigh-amylose cornstarch                 70(60% amylose content)Sodium caseinate(food additive grade) 30Glycerol (food additive grade)                 60______________________________________
Above mixture was milled in a two-roll mill at a surface temperature of 120� C., while successively adding suitable amounts of water on the one hand and simultaneously evaporating the water on the other hand, to form a uniform sheeting. The resulting sheeting was crushed by means of an impact crusher and admixed and 2 parts of lecithin (food additive grade) and left standing under a high humidity atmosphere at room temperature until the water content of the material reached 25% to obtain a granular, water-soluble, edible, thermoplastic molding composition. The granular molding composition thus obtained and favorable hopper-chargeability and showed also favorable moldability when tested by various molding methods such as extrusion, injection, inflation, and flow molding. The molding composition was stored in dark and cool place at a temperature below 10� C. It showed substantially no change after 6 months.
The said molding composition was continuously fed through a hopper into the barrel of an common extruder for common thermoplastic resin having a full flight screw (L/D = 20; compression ratio = 1.4) and milled under the following conditions: temperature inside the barrel = 120� - 160� C., revolution of screw = 30 - 100 rpm, pressure inside the barrel = 40 - 70 kg/cm2. The milled mass was continuously extruded through a hanger-type die (surface temperature = 100� C., opening gap at the die lip = 0.1 mm) and drawn by means of a cold takeoff roll, while controlling the take-off speed so as to keep the film thickness within the range from 60 to 100 μ. The extrudate was dried to a water content of 15 to 20% and taken off by means of a winder. The thus obtained water-soluble and edible thermoplastic extruded film was translucent, pale yellow in color, flexible at 20% R.H., and resistant to bleeding and blocking at R.H. 80%. When stored in dark place in a tightly closed polyethylene bag at a temperature below 10� C. for 6 months, the film showed no change at all.
Table 2______________________________________Relative humidity, %          20      45      65    80______________________________________Moisture content, %          5       10      15    35Dimensional change, %          7       5       2     0Tensile strength, kg/mm2          2.5     1.7     0.8   0.6Tensile modulus of          100     70      20    10elasticity, kg/mm2Elongation, %  10      20      35    50Tear strength, kg/mm2     2.0Folding endurance,          130     250     500   1,000numberHeat-sealability, second 100� C.          3       1.5     1.0   1.0 110� C.          2.5     1.5     1.0   0.5 130� C.          2       1.0     1.0   0.5          StandWater-solubility, second          still           Stirred______________________________________ 10� C.  75 - 160        60 - 125 20� C. 30 - 50         20 - 33 30� C.  7 - 15          5 - 10 40� C.  3 - 12         2 - 8Gas permeability,*cc/m2 � 24 hr. � atm. � 60______________________________________&#956; Oxygen        130 Nitrogen      12 Carbon dioxide          200______________________________________ Note: Extruded film, 60 &#956;  in thickness, was used in measurement of gas permeability.
The molding composition obtained above was automatically supplied to the barrel of an injection molding machine for common thermoplastic resin and plastified under the following conditions: temperature inside the barrel: 30� - 50� C. (water cooling) at the part below the hopper, 120� - 160� C. at middle part, 160� - 200� C. at front part. The molten mass was injected from the barrel under an injection pressure of 20 - 100 kg/cm2 into the mold cavity at 60� - 90� C. to obtain a water-soluble, edible, thermoplastic injection-molded article. This molded article was translucent, pale yellow in color, not subject to static charge, oil resistant, heatsealable, and difficulty permeable to oxygen gas. The article was found useful as a container for edible oils and butter and as a capsule shell for pharmaceutical preparations.
Table 3______________________________________          Example                 Example  Example          2      3        4______________________________________High-amylose cornstarch,parts (Amylose content,            50       50       5075%)Sodium caseinate, parts            40       40       40Glycerol, parts  60       60       60Hydroxyethylated starch,            10       --       --partsCarboxymethylated starch,            --       10       --partsStarch phosphate, parts            --       --       10Gum arabic, parts            --       --        2______________________________________
The molding compositions obtained in Examples 2 to 4 were extrusion-molded under the same conditions as in Example 1. The molded articles obtained were nearly the same in appearance and physical properties. The extruded films, each 100 μ in thickness, obtained from the molding compositions of Examples 2, 3, and 4 showed tensile strengths of 1.3 to 1.6 kg/cm2 and elongations of 18 to 23% at 20% R.H.
______________________________________               PartsHigh-amylose cornstarch(amylose content, 20%;                 40moisture content, 10%)Sodium caseinate (food additivegrade; moisture content, 10%                 40Glycerol (food additive grade)                 60Gelatin-sodium        20Lecithin               5______________________________________
The above ingredients were mixed in a Henschel mixer (800 to 1,200 rpm) at 40� to 70� C., while adding water successively to adjust the moisture content to 20%, to obtain a water-soluble and edible thermoplastic molding composition in the form of fine granule. The resulting fine granular molding composition has good hopper-chargability and moldability in various molding processes. The gelatin-sodium in the above formulation can be replaced by a salt of a protein concentrate obtained by extraction from soybean casein, wheat gluten, corn zein, or yeast and neutralized with alkalis to a pH of 6 to 8 to form a salt.
The molding composition obtained above was continuously fed through a hopper into the barrel of a vented exturder containing a dulmadge-type screw (L/D = 30; compression ratio = 1.8) and plastified and melted under the following conditions: temperature inside the barrel : 30� - 50� C. (water cooling) at the part below the hopper, 100� - 140� C. at middle part, 70� - 110� C. at front part; revolution speed of the screw, 60 - 200 rpm; pressure inside the barrel, 60 - 120 kg/cm2. The molten mass was continuously extruded through a die of the fishtail type (surface temperature, 70� - 90� C.; opening gap at the die lip, 0.05 mm) and drawn by means of a water-cooled roll, while controlling the take-off speed so as to keep the film thickness within the range from 40 to 60 μ. The extrudate was dried to a water content of 8 to 15% and taken off by means of a winder to obtain water-soluble and edible thermoplastic extruded film, 60 μ in thickness, which had a tensile strength of 1.5 kg/cm2 and an elongation of 15% at 10% R.H.
By using the molding composition obtained above, a translucent container, 0.5 mm in wall thickness, was molded by the injection-blow molding technique under the conditions similar to those in Example 1. This container disintegrated rapidly in water, whereas it withstood a refrigeration temperature of -20� C. when used as a container for an edible oil or margarine.
______________________________________               PartsHigh-amylose cornstarch                 40(amylose content, 50%)Sodium caseinate      30Glycerol              50Dried yeast           30Lecithin               5______________________________________
Table 4______________________________________          Example                 Example  Example          7      8        9______________________________________High-amylose cornstarch,parts (amylose content,            30       30       3085%)Casein-sodium, parts            70       70       70Glycerol, parts  30       30       30Lecithin, parts   1        1        1Ethylene glycol, parts            30       --       --Sorbitol, parts  --       30       --Maltitol, parts  --       --       30Sodium alginate, parts            --       10       --Water, parts     30       30       30______________________________________
The ingredients given in Table 4 were mixed in a blender at room temperature to form fine granules of a water content of 25%. By means of a conventional extruder for thermoplastic resins, provided with a full flight screw (L/D = 22, compression ratio = 1.5), the said fine granules were extruded into a rod, 3 mm in diameter, under the following conditions: temperature inside the cylinder, 120� - 160� C.; revolution speed of screw = 100 rpm; temperature of die, 80� - 110� C. The rod was cut into pellets to obtain a water-soluble and edible thermoplastic molding composition having favorable moldability.
Each of the molding compositions thus obtained was extruded through a tubing die of the rotary type under nearly the same conditions as in Example 1 and expanded by compressed air to form inflation film, 40 - 80 μ in thickness, which contained 15% of water and had nearly the same appearance and physical properties as those of the film obtained in Example 1. The film obtained was excellent especially in heat-sealability and bags were automatically made from the said film by means of a common heat-sealer at 110� to 150� C. with a cycle time of 0.5 to several seconds.
Table 5______________________________________            Ex.  Ex.     Ex.     Ex.            10   11      12      13______________________________________High-amylose cornstarch (amylose              70     70      70    70content, 50%), partsSodium caseinate, parts              30     30      30    30Glycerol, parts    30     30      30    30Lecithin, parts     1      1       1     1Sucrose monostearate, parts               1Glycerol monolaurate, parts                      1Sorbitol distearate, parts         1Maltitol monostearate, parts             1Mannan, parts                      5     2______________________________________
EXAMPLES 14 - 17
Table 6______________________________________             Ex.  Ex.     Ex.    Ex.             14   15      16     17______________________________________High-amylose cornstarch (amylose               40     40      40   40content, 53%), partsCasein-sodium, parts               40     40      30   40Glycerol, parts     40     40      40   40Lecithin, parts      2      2       2    2Wheat starch (amylose content, 25%),               20     --      --   --partsConverted &#945;-starch, parts               --     20      20   --Dextrin, parts      --     --      --   20Beer yeast, parts   --     --      10   --Sucrose monostearate, parts               --     --       2   --Water, parts        40     40      40   40______________________________________
Table 7______________________________________                Example                       Example                18     19______________________________________High-amylose cornstarch (amylose                  55       55content, 70%), partsLow-amylose cornstarch (amylosecontent, 5%), parts    10       --Dextrin, parts         --        5Starch phosphate, parts                  --        5Casein-potassium, parts                  --       10Gelatin-sodium, parts  25       25Yeast, sodium salt, parts                  10       --Glycerol, parts        60       40Mannitol, parts        --       20Sucrose monostearate, parts                  --        2Glycerol monostearate, parts                  --        2Lecithin, parts        10       --Sodium cellulose glycolate,                   5        5parts______________________________________
Table 8______________________________________             Ex.  Ex.     Ex.    Ex.             20   21      22     23______________________________________&#945;-Type high-amylose cornstarch                50     30     30   30(amylose content, 50%), partsCasein-sodium, parts 50     40     40   50Glycerol, parts      30     30     30   30Lecithin, parts      10     10     10   10Tapioca starch, parts                   20Waxy cornstarch (amylose content,  200%), partsFractionated potato starch (amylose                       20content, 100%), partsGelatin-sodium, parts              10Yeast, parts                10Ethylene glycol, parts      10          10Hydrogenated starch syrup, parts    5Sucrose distearate, parts                 1Glycerol trilaurate, parts   1Pectin, parts                2           2______________________________________
Table 9______________________________________Performance characteristicsof the extruded film obtainedin Example 20 (60 &#956; in thick-ness; relative humidity, 45%).Moisture content, %     12Tensile strength, kg/cm2                   1.8Tensile modulus of      25elasticity, kg/mm2Elongation, %           70                   Stand still:Water-solubility        15 - 20at 10� C., second                   Stirred:                   12 - 17______________________________________
Table 10______________________________________                Example                       Example                24     25______________________________________&#945;-Type potato starch (amylose                  18       18content, 20%), partsHigh-amylose cornstarch ethylether (amylose content, 60%),                   2       --partsHigh-amylose cornstarchphosphate (amylose content,                  --        260%), partsGelatin-sodium, parts  80       80Glycerol, parts        20       --Propylene glycol, parts                  --       10Sorbitan, parts        --       10Mannitol monolaurate, parts                   5        5Maltitol monostearate, parts                  --        5Pullulan, parts         2       --______________________________________
Table 11______________________________________           Example                  Example  Example           26     27       28______________________________________Tapioca starch (amylose             23       15       15content, 30%), parts&#945;-Type tapioca starch,             --        8       --partsDextrin, parts    --       --        4Carboxymethylstarch,             --       --        4partsCasein-sodium, parts             77       77       77Glycerol, parts   50       30       50Mannitol, parts   --       20       --Lecithin, parts    5        5        5Water, parts      30       30       30______________________________________
Following the procedure of Example 1, a water-soluble and edible thermoplastic molding composition of a water content of 28% was obtained from a mixture of ingredients of the same formulation as in Example 2, except that 40 parts of powdered casein and 8 parts of a 20-% aqueous solution of sodium hydroxide were used in place of 40 parts of powdered casein-sodium. The thus obtained molding composition had characteristic properties comparable to those of the molding composition obtained in Example 2. When similar variation of formulation was applied to the formulations of Examples 3 and 4, the characteristic properties of the resulting molding compositions were not much different from those of the compositions of original formulations.
A water-soluble and edible thermoplastic molding composition of a water content of 17% was obtained in the same manner as in Example 5, except that 40 parts of casein, 20 parts of gelatin, 10 parts of a 20-% aqueous solution of sodium hydroxide, and 5 parts of a 20-% aqueous dispersion of calcium hydroxide were used in place of 40 parts of casein-sodium and 20 parts of gelatin-sodium. The thus obtained molding composition had characteristic properties comparable to those of the molding composition obtained in Example 5. When similar variation of formulation was applied to the formulations of Examples 19 and 22, the characteristic properties of the resulting molding compositions were not much different from those of the compositions of original formulations.
A water-soluble and edible thermoplastic molding composition (28% water content) was obtained in the same manner as in Example 7, except that 65 parts of casein and 27 parts of an aqueous solution containing 20% of a mixture (1 : 1 by weight) of potassium hydroxide and potassium carbonate were used in place of 70 parts of casein-sodium. The thus obtained molding composition showed characteristic properties comparable to those of the molding composition obtained in Example 7. When similar variation of formulation was applied to the formulations of Examples 8 and 9, the characteristic properties of the resulting molding compositions were not much different from those of the compositions of original formulations.
A water-soluble and edible thermoplastic molding composition (22% water content) was obtained in the same manner as in Example 20, except that 49 parts of casein and 15 parts of a 20-% aqueous solution of sodium carbonate were used in place of 50 parts of casein-sodium. The thus obtained molding composition had characteristic properties comparable to those of the molding composition obtained in Example 20. When similar variation of formulation was applied to the formulation of Example 23, the characteristic properties of the resulting molding composition were not much different from those of the composition of original formulation.
A water-soluble and edible thermoplastic molding composition (35% water content) was obtained in the same manner as in Example 24, except that 80 parts of gelatin and 10 parts of a 20-% aqueous solution of sodium hydroxide were used in place of 80 parts of gelatin-sodium. The thus obtained molding composition had characteristic properties comparable to those of the composition obtained in Example 24. When similar variation of formulation was applied to the formulation of Example 25, the characteristic properties of the resulting molding composition were not much different from those of the composition of original formulation.
A water-soluble and edible thermoplastic molding composition (23% water content) was obtained in the same manner as in Example 26, except that 75 parts of casein and 15 parts of a 20-% aqueous solution of sodium hydroxide were used in place of 77 parts of casein-sodium. The thus obtained molding composition had characteristic properties comparable to those of the composition obtained in Example 26.
The extruded film obtained in Example 1 was exposed to the ultraviolet radiation for 3 minutes at room temperature. On examination of the exposed film, slight yellowing in color, emission of a peculiar odor, and a marked reduction in water-solubility were noticed (see Table 12).
Table 12______________________________________Change in water-solubilityTemperature Beforeof water, � C.       exposure     After exposure______________________________________ 0          6 - 15 min.  Swells, but remains                    insoluble50          3 sec. &gt;     5 sec. &gt;______________________________________
A water-soluble and edible thermoplastic molding composition (20% water content) was obtained in the same manner as in Example 5, except that 10 parts of common salt was added to the formulation. The resulting composition showed no significant change in moldability and in appearance and physical properties of the molded articles, except that the water-solubility at lower temperatures was markedly reduced as shown in Table 13.
Table 13______________________________________Change in water-solubilityTemperature                Exampleof water, � C.       Example 5      36______________________________________ 0          350 - 750 sec. Swelled but                      insoluble20          15 - 23 sec.   45 - 80 sec.40          2 - 7 sec.      3 - 10 sec.______________________________________
A water-soluble and edible thermoplastic molding composition (22% water content) was obtained in the same manner as in Example 7, except that 5 parts of lactic acid was added to the formulation. The resulting composition showed no substantial change in moldability and in appearance and physical properties of the molded articles, except that the water-solubility at lower temperatures was markedly reduced as shown in Table 14.
Table 14______________________________________Change in water-solubilityTemperatureof water, � C.       Example 7      Example 37______________________________________ 0          300 - 500 sec. Swelled but                      insoluble20          30 - 45 sec.   50 - 90 sec.40          3 - 8 sec.      4 - 15 sec.______________________________________
Following the procedure described in Example 7, a water-soluble and edible thermoplastic molding composition in granular form (20% water content) was obtained from a mixture of ingredients of the same formulation as in Example 20, except that 3 parts of sodium phosphate and 1 part of citric acid were further added to the formulation. The resulting composition showed no substantial change in moldability and in appearance and physical properties of the molded articles, except that in cold water below 10� C. the molded article remained insoluble, although swollen.
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