US2930671A - Process of producing cuprammonium cellulose articles - Google Patents
Process of producing cuprammonium cellulose articles Download PDFInfo
- Publication number
- US2930671A US2930671A US657502A US65750257A US2930671A US 2930671 A US2930671 A US 2930671A US 657502 A US657502 A US 657502A US 65750257 A US65750257 A US 65750257A US 2930671 A US2930671 A US 2930671A
- Authority
- US
- United States
- Prior art keywords
- cellulose
- spinning solution
- extruded
- cuprammonium
- ammonia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- 239000001913 cellulose Substances 0.000 title claims description 61
- 229920002678 cellulose Polymers 0.000 title claims description 61
- 238000000034 method Methods 0.000 title claims description 27
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 65
- 238000009987 spinning Methods 0.000 claims description 46
- 229910021529 ammonia Inorganic materials 0.000 claims description 32
- 229910052784 alkaline earth metal Chemical class 0.000 claims description 19
- 150000003839 salts Chemical class 0.000 claims description 16
- 229910052783 alkali metal Inorganic materials 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 229910052751 metal Inorganic materials 0.000 claims description 14
- 239000002184 metal Substances 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 150000001340 alkali metals Chemical class 0.000 claims description 3
- 150000001342 alkaline earth metals Chemical class 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 51
- -1 threads Substances 0.000 description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 13
- 229910052802 copper Inorganic materials 0.000 description 13
- 239000010949 copper Substances 0.000 description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 150000001242 acetic acid derivatives Chemical class 0.000 description 6
- 150000004675 formic acid derivatives Chemical class 0.000 description 6
- 150000002823 nitrates Chemical class 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 4
- 150000004820 halides Chemical class 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 3
- 230000001112 coagulating effect Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000004627 regenerated cellulose Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 150000003842 bromide salts Chemical class 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 150000008045 alkali metal halides Chemical class 0.000 description 1
- 229910001615 alkaline earth metal halide Inorganic materials 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910000365 copper sulfate Inorganic materials 0.000 description 1
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000001226 reprecipitation Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/02—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts
- D01F2/04—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from solutions of cellulose in acids, bases or salts from cuprammonium solutions
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/102—Silicates
- C10M2201/103—Clays; Mica; Zeolites
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/121—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms
- C10M2207/123—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of seven or less carbon atoms polycarboxylic
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
- C10M2207/14—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings
- C10M2207/141—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to carbon atoms of six-membered aromatic rings monocarboxylic
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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- C10M2207/22—Acids obtained from polymerised unsaturated acids
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- C10M2207/32—Esters of carbonic acid
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- C10M2207/40—Fatty vegetable or animal oils
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- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/40—Fatty vegetable or animal oils
- C10M2207/404—Fatty vegetable or animal oils obtained from genetically modified species
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
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- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/101—Condensation polymers of aldehydes or ketones and phenols, e.g. Also polyoxyalkylene ether derivatives thereof
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
- C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M2209/102—Polyesters
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- C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
- C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
- C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
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- C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
- C10M2227/09—Complexes with metals
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- C10N2010/00—Metal present as such or in compounds
- C10N2010/06—Groups 3 or 13
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- C10N2040/00—Specified use or application for which the lubricating composition is intended
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- C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
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- C10N2040/241—Manufacturing joint-less pipes
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- C10N2040/243—Cold working
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- C10N2040/244—Metal working of specific metals
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- C10N2040/245—Soft metals, e.g. aluminum
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- C10N2040/246—Iron or steel
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- C10N2040/247—Stainless steel
Definitions
- This invention relates to an improved process for the production of cellulose articles such as filaments, fibers, threads, films, ribbons, tapes and the like, and more particularly, the invention relates to an improved process of producing filamentary to filmaceous cellulose materials from a cuprammonium cellulose spinning solution.
- the cellulosic raw material is dissolved in an aqueous cuprammonium solution, the solution extruded or spun, e.g., as filaments or films, and the cellulose re-precipitated or coagulated by extrusion into a spin bath.
- monium solvent must consist of specific quantities or concentrations of copper (in cupric form) and ammonia in order for the cellulose to remain dissolved therein, and the aqueous spin bath, which may be acidic or basic, functions as a diluent to lower the concentration of ammemo. and copper to the point where the cellulose precipitates.
- the spin bath also serves to remove solvent from the precipitated filaments or films.
- the cuprammonium spinning solution is extruded into a funnel through which the spin bath is circulated, and the extruded and precipitated filaments are stretched as they pass through the funnel.
- the tensile strength of the resulting cellulosic articles can be increased by subjecting the so-called blue filaments leaving the funnel to a subsequent stretching or drawing. After stretching, the filaments or films are passed through a bath for washing and decopperizing. In order to further increase the tensile strength, the blue filaments leaving the funnel have been converted into a copper alkaline cellulose compound, and the filaments then stretched to a maximum of about 100% as they are passed through successive tartaric acid baths. In both of these methods, however, the filaments are stretched or drawn only after a substantially complete disintegration or separation of the cellulose from the cuprammonium'solution by water dilution and precipitation or coagulation of the cellulose. Even with the high stretch methods heretofore employed in which the filaments are gradually drawn in a coagulating or precipitating bath, the maximum tensile strengths which have been obtained are only about 2.5 grams per denier.
- One object of the invention is to provide an improved process for the production of cellulose filaments and films having higher tensile strength and a denser structure than could be previously accomplished.
- Another object of the invention is to provide a process of producing filamentary and filmaceous cellulosic articles of high tensile strength by a novel method of spinning or extruding a cuprammonium cellulose solution and stretching the coagulated product before regenerating the cellulose.
- Still another object of the invention is to provide a new and improved method of setting or coagulating a cuprammonium cellulose solution extruded in the form of filaments or films.
- the novel aqueous spin bath of the invention contains three essential components as follows:
- the cuprammonium cellulose spinning solution employed in the process of the invention can be prepared by well-known conventional method and preferably contains copper (in cupric form) in a concentration of from 2-4% and ammonia in a concentration of from about 4.5-7%.
- This spinning solution is extruded from a conventional spinning or casting head having an aperture or plurality of apertures to form the desired filament or film.
- filaments can be spun from holes having a diameter of 1 mm. or less, preferably 0.1-0.3 mm.
- the spinning solution is extruded in the desired shape or form directly into the novel spinning and stretching bath having a composition as specified by the invention. Stretching or drawing of the extruded spinning solution after coagulation'in the novel bath is carried out in the usual manner, e.g., by means of a godet roller or similar drawing device.
- the setting or coagulation of the cuprammonium cellulose solution is accomplished by the presence of the alkali metal or alkaline earth metal salts in the spin bath.
- the quantity or concentration of the setting agent or component (1) varies depending upon whether the alkali metal salts or the alkaline earth metal salts are employed. With alkali metal salts, a concentration of at least 2 mols/liter is preferably employed, and, alternatively, a concentration of at least 0.1 mol/liter of the alkaline earth metal is most advantageous.
- the setting agent can, if desired, consist of a mixture of alkali and alkaline earth metal salts.
- the minimum concentration of the setting agent is preferably selected such that the sum of the concentrations, expressed as percentages of the above-mentioned minimum concentrations of each class of salts, is at least equal to (See Example III below, for example.)
- the minimum concentration is Obtained when the formula 100[a/2'+l2/0.1] isequal to at least 00, wherein a is the number of mols per liter of the alkali metal salt and'b is the number of mols per liter of the alkaline earth metal salt, based upon the'aqueous spin bath.
- alkali and alkaline earth metal salts are especially useful: the halides, e.g., chlorides and bromides, nitrates, formates and acetates of sodium and potassium. If only alkali metal salts are employed, then the alkali sulfates and carbonates may also be used.
- the optimum concentration of free ammonia, component (2), ofv the spin bath is that which corresponds or is about equal to the concentration of ammonia in the spinning solution, i.e., about 3 to 4 mols/liter.
- suitable ammonia complex-forming metal salts are known, and the following are especially useful as component (3) of the novel spin bath: the halides, e.g., chlorides and bromides, nitrates, formates and acetates of copper, zinc, cadmium, cobalt and nickel.
- the sulfates and carbonates of the same metals can be employed.
- the setting agent, component (1) causes the extruded spinning solution to coagulate or set
- the free ammonia and complex-forming metal salts, components (2) and (3) act to repress or substantially suppress the separation or disintegration of cellulose from the cuprammonium solution.
- the stretch capacity of the extruded filaments or films is at its maximum when the disintegration of the spinning solution, i.e., separation of cellulose from the cuprammonium solvent, is completely prevented.
- This state or-condition is substantially achieved when employing the above-mentioned optimum concentrations of components (2) and (3). Higher concentrations of these compounds in the spin bath is'pejrmissible, but no further improvement of the stretchingcapacity of the filaments or films can be achieved thereby.
- the present invention permits the extruded filamentary to filmaceous materials to be stretched or'elongated to from 50% to as high as 350%.
- the structure of thefinished product isthereby made considerably more dense, and it is possible to achieve high values of tensile strength.
- the invention is capable of providing filaments having dry tensile strength values of about 3 to 5 grams/denier and wet-strength values of about 2 to 4 grams/denier, together with a wet to dry elongation value of 5 to 12%, as well as films with a strength of kg./mm.
- Example I A cuprammonium cellulose solution having 9% cellulose, 6.5% ammonia and 3.8% of copper is spun through a nozzle of 0.1 mm. in diameter into a spin bath that contains 0.8 mol/liter of calcium chloride, 3.7 mols/liter of ammonia and 0.1 mol/ liter of copper chloride.
- the singlestrand filament is set or coagulated by the spin bath and is then subjected to a stretch or elongation of 150%. After washing and decopperizing with hydrochloric acid, a single-strand filament is obtained with a titer of 5 denier. Its properties are: dry strength, 5 .2 grams/denier; wet
- Example II A spinning solution having the same composition as Example I is extruded through a 24-hole nozzle into a spin bath which contains 0.6 mol/ liter (600% of the minimum quantity) of calcium chloride, 1 moi/liter (50% of the minimum quantity) of sodium chloride (altogether 650%), 2 mols/liter of ammonia, and 0.1 mol/liter of copper chloride. Theset or solidified thread is stretched by and acidified with hydrochloric acid.
- the resuiting filamentary material has a titer of 60 denier, a dry elongation of 10%, and a Wet elongation of 8%. The dry tensile strength is 3.4 grams/denier, and the wet strength is 2.3 grams/denier.
- Example 1V A spinning solution of the same composition as Example I is extruded through a l6-hole nozzle into a spin bath that contains 4 mols/liter of sodium chloride, 0.2 mol/liter of ammonia, and 0.01 moi/liter of copper sulfate.
- a titer of 40 denier a dry strength of 3.2 grams/denier; a wet strength of 2.3 grams/denier; a dry elongation of 11%; and a wet elongation of 8%.
- a process for the production of cellulose articles such as filaments and films from a cuprammonium cellulose spinning solution comprising: extruding a cuprammonium spinning solution in an aqueous spin bath which contains (1) a setting agent selected from at least one member of the group consisting of alkali metal and alkaline earth metal salts in a quantity sufficient to set the extruded spinning solution, (2) from 2 up to about 8 mols/liter of free ammonia, and (3) an ammonia complex-forming metal salt, said ammonia and said ammonia complex-forming metal salt being present in a quantity sulficient to prevent substantial separation of cellulose from the extruded cuprammonium cellulose spinning solution; and stretching the extruded and coagulated product prior to separating the cellulose therefrom.
- a setting agent selected from at least one member of the group consisting of alkali metal and alkaline earth metal salts in a quantity sufficient to set the extruded spinning solution, (2) from 2 up to about 8 mols/liter of free am
- the setting agent is a mixture of an alkali metal salt and an alkaline earth metal salt dissolved in the aqueous spin bath in an amount such that 100[a/2+b/0.1] equals at least 100 wherein a is the number of mols/liter of the alkali metal salt and b is the number of mols/ liter of the alkaline earth metal salt.
- the setting agent is an alkali metal salt selected from the group consisting of alkali metal halides, nitrates, formates and acetates, sulfates and carbonates.
- alkaline earth metal salt is a member of the group consisting of alkaline earth metal halides, nitrates, formates and acetates.
- ammonia complex-forming metal salt is a member of the group consisting of the halides, nitrates, formates, acetates, sulfates and carbonates of copper, zinc, cadmium, cobalt and nickel in a concentration in the aqueous spin bath of up to about 0.1 mol/liter, and wherein the setting agent is an alkali metal salt.
- ammonia complex-forming metal salt is present in the aqueous spin bath in a molar concentration about equivalent to the corresponding molar concentration of the bivalent copper not bound to cellulose in the cuprammonium cellulose spinning solution.
- a cuprammonium cellulose spinning solution which contains the components 1) a setting agent selected from at least one member of the group consisting of alkali metal salts and alkaline earth metal salts in a minimum concentration based upon the aqueous spin bath such that l00[a/2+b/ 0.l] equals at least 100 wherein a is the number of mols/liter of the alkali metal salt and b is the number of mols/liter of the alkaline earth metal salt,
- component (1) being present in a quantity suflicient to coagulate the extruded spinning solution and components (2) and (3) being present in a quantity suflicient to prevent substantial separation of cellulose from the extruded spinning solution; stretching the extruded and coagulated spinning solution from 50 to 350% prior to separation of the cellulose therefrom; and washing and decopperizing the extruded, coagulated and stretched product in an acid aqueous bath to regenerate cellulose.
- cupric chloride in a molar concentration about equivalent to the corresponding molar concentration of the bivalent copper not bound to cellulose in the cuprammonium cellulose spinning solution
- components (2) and (3) being present in a quantity sufficient to prevent substantial separation of cellulose from the extruded spinning solution in the spin bath; stretching the extruded and coagulated spinningsolution from to' 350% prior to separation of the cellulose therefrom; and washing and decopperizing the extruded,
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Glass Compositions (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEB40203A DE1053719B (de) | 1956-05-11 | 1956-05-11 | Verfahren zur Herstellung von Faeden und Filmen aus Kupferoxydammoniakcelluloseloesung |
Publications (1)
Publication Number | Publication Date |
---|---|
US2930671A true US2930671A (en) | 1960-03-29 |
Family
ID=6966019
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US657502A Expired - Lifetime US2930671A (en) | 1956-05-11 | 1957-05-07 | Process of producing cuprammonium cellulose articles |
Country Status (7)
Country | Link |
---|---|
US (1) | US2930671A (de) |
BE (1) | BE555517A (de) |
CH (1) | CH360760A (de) |
DE (1) | DE1053719B (de) |
FR (1) | FR1170088A (de) |
GB (1) | GB815189A (de) |
NL (2) | NL216995A (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4164437A (en) * | 1976-06-22 | 1979-08-14 | Akzo N.V. | Method of producing dialyzing membrane |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2319428A (en) * | 1940-10-05 | 1943-05-18 | Imp Rayon Corp | Rayon manufacture |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE286297C (de) * | ||||
DE225161C (de) * | ||||
DE498158C (de) * | 1925-03-26 | 1930-05-19 | J P Bemberg Akt Ges | Verfahren zur Herstellung von Kunstfaeden aus Kupferoxydammoniakcelluloseloesungen |
DE682884C (de) * | 1937-02-27 | 1939-10-24 | I G Farbenindustrie Akt Ges | Verfahren zum Verspinnen von Kupferoxydammoniakcelluloseloesungen |
-
0
- NL NL100700D patent/NL100700C/xx active
- BE BE555517D patent/BE555517A/xx unknown
- NL NL216995D patent/NL216995A/xx unknown
-
1956
- 1956-05-11 DE DEB40203A patent/DE1053719B/de active Pending
-
1957
- 1957-03-27 FR FR1170088D patent/FR1170088A/fr not_active Expired
- 1957-04-23 GB GB12953/57A patent/GB815189A/en not_active Expired
- 1957-05-07 US US657502A patent/US2930671A/en not_active Expired - Lifetime
- 1957-05-09 CH CH360760D patent/CH360760A/de unknown
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2319428A (en) * | 1940-10-05 | 1943-05-18 | Imp Rayon Corp | Rayon manufacture |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4164437A (en) * | 1976-06-22 | 1979-08-14 | Akzo N.V. | Method of producing dialyzing membrane |
Also Published As
Publication number | Publication date |
---|---|
NL100700C (de) | |
FR1170088A (fr) | 1959-01-08 |
BE555517A (de) | |
GB815189A (en) | 1959-06-17 |
DE1053719B (de) | 1959-03-26 |
NL216995A (de) | |
CH360760A (de) | 1962-03-15 |
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