US2702230A - Cellulose acetate spinning process - Google Patents

Cellulose acetate spinning process Download PDF

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US2702230A
US2702230A US197516A US19751650A US2702230A US 2702230 A US2702230 A US 2702230A US 197516 A US197516 A US 197516A US 19751650 A US19751650 A US 19751650A US 2702230 A US2702230 A US 2702230A
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filamentary materials
cellulose
cellulose acetate
coagulating medium
materials
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US197516A
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Francois J Olmer
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Celanese Corp
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Celanese Corp
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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
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate

Definitions

  • This invention relates to filamentary materials and relates more particularly to a process for the production of filamentary materials having a basis of cellulose acetate or other organic acid ester of cellulose.
  • a further object of this invention isvtoyprovide an improved process for the production of filamentary materials wherein a solution of cellulose acetate or other organic acid ester of cellulose is spun into a coagulating medium comprising a latent solvent incapable of dissolving the cellulose ester, but capable of swelling it to a considerable extent.
  • a still further object of this invention is to provide an improved process for the production of filamentary materials wherein a solution of cellulose acetate or other organic acid ester of cellulose is spun into a coagulating medium comprising a mixture of carbon tetrachloride and methylene chloride.
  • Another object of this invention is to provide a process for the production of filamentary materials wherein a solution of cellulose acetate or other organic acid ester of cellulose is spun into a coagulating medium comprising a mixture of carbon tetrachloride and methylene chloride and the filamentary materials are passed, while still wet with the coagulating medium, into a saponification bath.
  • filamentary materials having a basis of.cellulose acetate or other organic acid ester of cellulose In the production of filamentary materials having a basis of.cellulose acetate or other organic acid ester of cellulose by the wet-spinning process, a solution of the filament-forming material in a suitable solvent is pumped or otherwise forced through a spinning jet, having at least one spinning orifice therein, into a liquid coagulating medium which causes the filament-forming material to coagulate or set and which extracts the solvent therefrom. It has previously been proposed to increase the tenacity of the filamentary materials produced in this manner by stretching said materials during the, spinning operation while they are still in a relatively plastic state. In this way, it is possible to produce filamentary materials having tenacities of from 2 to 5 or more grams per denier.
  • the increase in the tenacity of the filamentary materials is accompanied by a reduction in their elongation, so that it is diflicult to weave, knit or otherwise prgcess said high-tenacity filamentary materials into textile a rics.
  • a solution of cellulose acetate or other organic acid ester of cellulose is pumped or otherwise forced through a spinning jet, having at least one spinning orifice therein, into a coagulating medium comprising a mixture of the type specified above.
  • the filamentary materials formed in this manner are stretched while they are still in a relatively plastic state,
  • a spinning solutionor dope is prepared by dissolving cellulose acetate or other organic acid ester of cellulose in a suitable solvent such as, for example, acetone, acetonewater mixtures, 98:2% by -weight or 95:5% by weight, preferably in an amount sutficient to yield spinning dope containing from about 18 to 28% by weight of the filament-forming material.
  • the spinning dope after being filtered to remove therefrom all solid impurities, is spun into a coagulating medium containing, for example, fr om about 10 to 25% by volume of carbon tetrachloride, the remainder being methylene chloride.
  • the filament forming material is caused to set or gel and the solvent is extracted therefrom by the coagulating medium.
  • Other coagulating media that may be employed include, for example, dichloroethane and tetrachloroethane alone; ethylene chloride, alone, or admixed with carbon tetrachloride (95 :5% -by weight); chloroform admixed with carbon tetrachloride (80:20% to :10% by weight) and methylene chloride admixed with'benzene, toluene, -cyclohexane and the like.
  • the filamentary materials While the filamentary materials are still in a relatively plastic state, they are stretched to increase their length by about 1000 to 5000%.
  • the stretching may be effected by passing the filamentary materials over a number of rollers immersed in the coagulating medium, each successive roller having a higher peripheral speed than the preceding roller.
  • the stretching is effected by means of a positively driven roller which draws the filamentary materials from the coagulating medium at the proper speed. After the filamentary materials emerge from the coagulating medium they are dried, following which they may be twisted and wound onto a textile package or otherwise treated to prepare them for further use.
  • the coagulating medium is advantageously maintained at a temperature of from about 0 to 30 C. depending upon its composition.
  • a temperature of from about 0 to 30 C. depending upon its composition When the coagulating'medium is employed at the higher temperatures within this range,
  • the concentration of any cellulose ester solvent, such as methylene chloride, therein should be kept below the value at which excessive softening of the filamentary materials will take place, which, when multi-filament materials are being produced, may cause thti:1 individual filaments thereof to coalesce, one with the 0 er.
  • the saponification may be effected by treating the dried filamentary materials with a suitable saponification bath, it has been found that the saponification may be effected more rapidly and more uniformly by passing the filamentary materials through the saponification bath While they are still wet with the coagulating medium.
  • the filamentary materials may be passed directly from one container holding the vcoagulating medium into another container holding the saponification bath, care being taken to avoid any substantial evaporation of the coagulating medium from the filamentary materials as said materials pass from one container to the other.
  • a preferred method for efiecting the saponification is to float a saponification bath immiscible with the coagulating medium on the coagulating medium so that the filamentary materials will pass through said saponification bath as they emerge from the coagulating medium. In this way,
  • the filamentary materials are withdrawn from the saponification bath and are washed to remove therefrom the products of saponification and the saponification bath and dried, following which they may be twisted and wound onto a textile package or otherwise treated to prepare them for further use.
  • the saponification bath there may be employed, for example, aqueous solutions of alkaline materials such as sodium hydroxide,potassium hydroxide or ammonium hydroxide, to which solutions there may be added buffering salts such as sodium acetate, potassium acetate or ammonium acetate to make more uniform the action of said baths.
  • alkaline materials such as sodium hydroxide,potassium hydroxide or ammonium hydroxide
  • buffering salts such as sodium acetate, potassium acetate or ammonium acetate to make more uniform the action of said baths.
  • filamentary materials having a basis of cellulose acetate, which is commercially the most important organic acid ester of cellulose at the present time. It may also be employed for the production of filamentary materials having a basis of other organic acid esters of cellulose, such as, cellulose propionate, cellulose butyrate, cellulose acetate propionate and cellulose acetate butyrate.
  • Example I Dope containing 26% by weight of cellulose acetate dissolved in acetone is spun into a coagulating medium containing 85% by volume of methylene chloride and 15% by volume of carbon tetrachloride maintained at a temperature of 25 C.
  • the filamentary materials travel-
  • Example 11 Dope containing 25% by weight of cellulose acetate, having an acetyl value of 54.6%, calculated as acetic acid, dissolved in acetone, is spun into a coagulating medium. containing 82.5% by volume of methylene chloride and 17.5 by volume of carbon tetrachloride maintained at a temperature of 25 C.
  • the filamentary materials travel through said coagulating medium for a distance of 9 inches and are stretched to increase their length 2200%.
  • the filamentary materials then travel through a 3 inch layer of 20% aqueous ammonium hydroxide which is floate'd upon the surface of the coagulat- 4 ing medium. Upon emerging from the coagulating medium, the filamentary materials are washed and dried and are then wound onto a spool at a rate of 81 meters per minute.
  • the filamentary materials are partially saponified and have an average acetyl value of 48%, calculated as acetic acid, and exhibit a tenacity of 3.24 grams per denier and an elongation of 16.4% at the breaking point.
  • Example III The process set forth in Example I is repeated, employing as a coagulating medium a mixture of 95% by weight of ethylene chloride and 5% by weight of carbon tetrachloride, and taking up the filamentary materials at a rate of 97 meters per minute.
  • the filamentary materials exhibit a tenacity of 2 grams per denier and an elongation of 43% at the breaking point.
  • Example I V' The process set forth in Example I is repeated, employing as a coagulating medium a mixture of 82.5% by weight of methylene chloride and 17.5% by weight of cyclohexane, and taking up the filamentary materials at a rate of 68 meters per minute.
  • the filamentary materials exhibit a tenacity of 3.5 grams per denier and an elongation of 22% at the breaking point.
  • Process for the production of filamentary materials which comprises spinning a solution containing 25% by weight of cellulose acetate having an acetyl value of 54.6% dissolved in acetone into a coagulating medium maintained at 25 C. and containing 82.5% by volume of methylene chloride and 17.5% by volume of carbon tetrachloride, stretching the filamentary materials to increase their length 2200% while they travel through said coagulating medium for a distance of 9 inches, then passing said filamentary materials through a 3 inch layer of 20% aqueous ammonium hydroxide which isfioated 0n the coagulating medium to reduce the average acetyl value of the cellulose acetate to 48%, washing and drying the filamentary materials, and taking up the filamentary materials at a rate of 81 meters per minute.

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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)

Description

United States Patent CELLULOSE ACETATE SPINNING PROCESS Francois I. Olmer, Morristown, N. 1., asslgnor to Celanese Corporation of America, New York, N. Y., a corporation of Delaware No Drawing. Application November 24, 1950,
Serial No. 197,516
1 Claim. (CI. 18-54) This invention relates to filamentary materials and relates more particularly to a process for the production of filamentary materials having a basis of cellulose acetate or other organic acid ester of cellulose.
It is an important object of this invention to provide a process for the production of high tenacity filamentary materials having a basis of cellulose. acetate or other organic acid ester of cellulose.
A further object of this invention isvtoyprovide an improved process for the production of filamentary materials wherein a solution of cellulose acetate or other organic acid ester of cellulose is spun into a coagulating medium comprising a latent solvent incapable of dissolving the cellulose ester, but capable of swelling it to a considerable extent.
A still further object of this invention is to provide an improved process for the production of filamentary materials wherein a solution of cellulose acetate or other organic acid ester of cellulose is spun into a coagulating medium comprising a mixture of carbon tetrachloride and methylene chloride. I I
Another object of this invention is to provide a process for the production of filamentary materials wherein a solution of cellulose acetate or other organic acid ester of cellulose is spun into a coagulating medium comprising a mixture of carbon tetrachloride and methylene chloride and the filamentary materials are passed, while still wet with the coagulating medium, into a saponification bath.
Other objects of this invention will be apparent from the following detailed description and claim.
In the production of filamentary materials having a basis of.cellulose acetate or other organic acid ester of cellulose by the wet-spinning process, a solution of the filament-forming material in a suitable solvent is pumped or otherwise forced through a spinning jet, having at least one spinning orifice therein, into a liquid coagulating medium which causes the filament-forming material to coagulate or set and which extracts the solvent therefrom. It has previously been proposed to increase the tenacity of the filamentary materials produced in this manner by stretching said materials during the, spinning operation while they are still in a relatively plastic state. In this way, it is possible to produce filamentary materials having tenacities of from 2 to 5 or more grams per denier. However, the increase in the tenacity of the filamentary materials is accompanied by a reduction in their elongation, so that it is diflicult to weave, knit or otherwise prgcess said high-tenacity filamentary materials into textile a rics.
l have now discovered that by spinning a solution of cellulose acetate or other organic acid ester of cellulose into a coagulating medium comprising a latent solvent incapable of dissolving the cellulose ester, but capable of swelling it to a considerable extent, such as a mixture of carbon tetrachloride and methylene chloride, and stretching said filamentary materials while they are still in a relatively plastic state, it is possible to obtain products having both a high tenacity and a good elongation which may be converted without difficulty into textile fabrics. Thus, in accordance with the present invention a solution of cellulose acetate or other organic acid ester of cellulose is pumped or otherwise forced through a spinning jet, having at least one spinning orifice therein, into a coagulating medium comprising a mixture of the type specified above. The filamentary materials formed in this manner are stretched while they are still in a relatively plastic state,
2,702,230 Patented Feb. 15, 1955 stretched during their production, the higher the degree of stretch the higher the tenacity and the lower the elongation of the final product.
In' carrying out the process of the present invention, a spinning solutionor dope is prepared by dissolving cellulose acetate or other organic acid ester of cellulose in a suitable solvent such as, for example, acetone, acetonewater mixtures, 98:2% by -weight or 95:5% by weight, preferably in an amount sutficient to yield spinning dope containing from about 18 to 28% by weight of the filament-forming material. The spinning dope, after being filtered to remove therefrom all solid impurities, is spun into a coagulating medium containing, for example, fr om about 10 to 25% by volume of carbon tetrachloride, the remainder being methylene chloride. As the spinning dope enters the coagulating medium, the filament forming material is caused to set or gel and the solvent is extracted therefrom by the coagulating medium. Other coagulating media that may be employed include, for example, dichloroethane and tetrachloroethane alone; ethylene chloride, alone, or admixed with carbon tetrachloride (95 :5% -by weight); chloroform admixed with carbon tetrachloride (80:20% to :10% by weight) and methylene chloride admixed with'benzene, toluene, -cyclohexane and the like.
While the filamentary materials are still in a relatively plastic state, they are stretched to increase their length by about 1000 to 5000%. The stretching may be effected by passing the filamentary materials over a number of rollers immersed in the coagulating medium, each successive roller having a higher peripheral speed than the preceding roller. Preferably, however, the stretching is effected by means of a positively driven roller which draws the filamentary materials from the coagulating medium at the proper speed. After the filamentary materials emerge from the coagulating medium they are dried, following which they may be twisted and wound onto a textile package or otherwise treated to prepare them for further use.
The coagulating medium is advantageously maintained at a temperature of from about 0 to 30 C. depending upon its composition. When the coagulating'medium is employed at the higher temperatures within this range,
say above about 25 C., the concentration of any cellulose ester solvent, such as methylene chloride, therein should be kept below the value at which excessive softening of the filamentary materials will take place, which, when multi-filament materials are being produced, may cause thti:1 individual filaments thereof to coalesce, one with the 0 er.
To improve the tenacity and/or to modify the dyeing and other properties of the filamentary materials prepared in the manner set forth above, it is frequently desirable to saponify the cellulose acetate or other organic acid ester of cellulose, either partially or completely. While the saponification may be effected by treating the dried filamentary materials with a suitable saponification bath, it has been found that the saponification may be effected more rapidly and more uniformly by passing the filamentary materials through the saponification bath While they are still wet with the coagulating medium. Thus, the filamentary materials may be passed directly from one container holding the vcoagulating medium into another container holding the saponification bath, care being taken to avoid any substantial evaporation of the coagulating medium from the filamentary materials as said materials pass from one container to the other. A preferred method for efiecting the saponification is to float a saponification bath immiscible with the coagulating medium on the coagulating medium so that the filamentary materials will pass through said saponification bath as they emerge from the coagulating medium. In this way,
agcaaao the escr e of the coagulating medium from the filamentary materials before they enter the saponificatlon bath 18 substantially avoided and, in addition, the saponification bath acts to seal the coagulating medium from the atmosphere ereby minimizing the loss of said medium through evaporation. When the saponification has progressed to the desired extent, the filamentary materials are withdrawn from the saponification bath and are washed to remove therefrom the products of saponification and the saponification bath and dried, following which they may be twisted and wound onto a textile package or otherwise treated to prepare them for further use.
As the saponification bath there may be employed, for example, aqueous solutions of alkaline materials such as sodium hydroxide,potassium hydroxide or ammonium hydroxide, to which solutions there may be added buffering salts such as sodium acetate, potassium acetate or ammonium acetate to make more uniform the action of said baths.
The process of this invention will now be described specifically in connection with the production of filamentary materials, having a basis of cellulose acetate, which is commercially the most important organic acid ester of cellulose at the present time. It may also be employed for the production of filamentary materials having a basis of other organic acid esters of cellulose, such as, cellulose propionate, cellulose butyrate, cellulose acetate propionate and cellulose acetate butyrate.
The following examples are given to illustrate this invention further.
Exqmple I Dope containing 26% by weight of cellulose acetate dissolved in acetone is spun into a coagulating medium containing 85% by volume of methylene chloride and 15% by volume of carbon tetrachloride maintained at a temperature of 25 C. The filamentary materials travel- Example 11 Dope containing 25% by weight of cellulose acetate, having an acetyl value of 54.6%, calculated as acetic acid, dissolved in acetone, is spun into a coagulating medium. containing 82.5% by volume of methylene chloride and 17.5 by volume of carbon tetrachloride maintained at a temperature of 25 C. The filamentary materials travel through said coagulating medium for a distance of 9 inches and are stretched to increase their length 2200%. The filamentary materials then travel through a 3 inch layer of 20% aqueous ammonium hydroxide which is floate'd upon the surface of the coagulat- 4 ing medium. Upon emerging from the coagulating medium, the filamentary materials are washed and dried and are then wound onto a spool at a rate of 81 meters per minute. The filamentary materials are partially saponified and have an average acetyl value of 48%, calculated as acetic acid, and exhibit a tenacity of 3.24 grams per denier and an elongation of 16.4% at the breaking point.
Example III The process set forth in Example I is repeated, employing as a coagulating medium a mixture of 95% by weight of ethylene chloride and 5% by weight of carbon tetrachloride, and taking up the filamentary materials at a rate of 97 meters per minute. The filamentary materials exhibit a tenacity of 2 grams per denier and an elongation of 43% at the breaking point.
Example I V' The process set forth in Example I is repeated, employing as a coagulating medium a mixture of 82.5% by weight of methylene chloride and 17.5% by weight of cyclohexane, and taking up the filamentary materials at a rate of 68 meters per minute. The filamentary materials exhibit a tenacity of 3.5 grams per denier and an elongation of 22% at the breaking point.
It is to be understood that the foregoing detailed description is given merely by way of illustration and that many variations may be made therein without departing from the spirit of my invention.
Having described my invention, what I desireto secure by Letters Patent is:
Process for the production of filamentary materials which comprises spinning a solution containing 25% by weight of cellulose acetate having an acetyl value of 54.6% dissolved in acetone into a coagulating medium maintained at 25 C. and containing 82.5% by volume of methylene chloride and 17.5% by volume of carbon tetrachloride, stretching the filamentary materials to increase their length 2200% while they travel through said coagulating medium for a distance of 9 inches, then passing said filamentary materials through a 3 inch layer of 20% aqueous ammonium hydroxide which isfioated 0n the coagulating medium to reduce the average acetyl value of the cellulose acetate to 48%, washing and drying the filamentary materials, and taking up the filamentary materials at a rate of 81 meters per minute.
References Cited in the file of this patent
US197516A 1950-11-24 1950-11-24 Cellulose acetate spinning process Expired - Lifetime US2702230A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2838365A (en) * 1955-12-21 1958-06-10 Eastman Kodak Co Dry spinning process
US2988418A (en) * 1954-10-13 1961-06-13 British Celanese Manufacture of artificial filaments, films and like shaped articles of cellulose triacetate
US3056163A (en) * 1955-05-18 1962-10-02 American Viscose Corp Spinneret
US3071806A (en) * 1958-01-29 1963-01-08 Celanese Corp Wet spinning column and process
US4543409A (en) * 1982-12-15 1985-09-24 Akzo Nv Water-insoluble fibers of cellulose acetate, cellulose propionate and cellulose butyrate with an extremely high absorptive capacity for water and physiological liquids
US11492757B2 (en) * 2018-08-23 2022-11-08 Eastman Chemical Company Composition of matter in a post-refiner blend zone
US11512433B2 (en) 2018-08-23 2022-11-29 Eastman Chemical Company Composition of matter feed to a head box

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1119155A (en) * 1911-07-26 1914-12-01 Nl Kunstzijdefabriek Nv Manufacture of artificial thread.
US1456781A (en) * 1919-05-14 1923-05-29 Du Pont Process of recovering cellulose acetate from solutions thereof
US1906041A (en) * 1926-12-28 1933-04-25 Ruthaldo Company Inc Method for the formation of filaments and the like of a cellulose ester
US1920188A (en) * 1929-01-18 1933-08-01 Celanese Corp Production of artificial materials
US2075027A (en) * 1931-10-21 1937-03-30 Dreyfus Henry Manufacture and treatment of artificial silk and like products
US2075430A (en) * 1935-03-07 1937-03-30 Dreyfus Henry Manufacture or treatment of artificial materials

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1119155A (en) * 1911-07-26 1914-12-01 Nl Kunstzijdefabriek Nv Manufacture of artificial thread.
US1456781A (en) * 1919-05-14 1923-05-29 Du Pont Process of recovering cellulose acetate from solutions thereof
US1906041A (en) * 1926-12-28 1933-04-25 Ruthaldo Company Inc Method for the formation of filaments and the like of a cellulose ester
US1920188A (en) * 1929-01-18 1933-08-01 Celanese Corp Production of artificial materials
US2075027A (en) * 1931-10-21 1937-03-30 Dreyfus Henry Manufacture and treatment of artificial silk and like products
US2075430A (en) * 1935-03-07 1937-03-30 Dreyfus Henry Manufacture or treatment of artificial materials

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2988418A (en) * 1954-10-13 1961-06-13 British Celanese Manufacture of artificial filaments, films and like shaped articles of cellulose triacetate
US3056163A (en) * 1955-05-18 1962-10-02 American Viscose Corp Spinneret
US2838365A (en) * 1955-12-21 1958-06-10 Eastman Kodak Co Dry spinning process
US3071806A (en) * 1958-01-29 1963-01-08 Celanese Corp Wet spinning column and process
US4543409A (en) * 1982-12-15 1985-09-24 Akzo Nv Water-insoluble fibers of cellulose acetate, cellulose propionate and cellulose butyrate with an extremely high absorptive capacity for water and physiological liquids
US11492757B2 (en) * 2018-08-23 2022-11-08 Eastman Chemical Company Composition of matter in a post-refiner blend zone
US11512433B2 (en) 2018-08-23 2022-11-29 Eastman Chemical Company Composition of matter feed to a head box

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