US1997753A - Manufacture of artificial threads from cellulose esters or cellulose ethers - Google Patents
Manufacture of artificial threads from cellulose esters or cellulose ethers Download PDFInfo
- Publication number
- US1997753A US1997753A US358762A US35876229A US1997753A US 1997753 A US1997753 A US 1997753A US 358762 A US358762 A US 358762A US 35876229 A US35876229 A US 35876229A US 1997753 A US1997753 A US 1997753A
- Authority
- US
- United States
- Prior art keywords
- cellulose
- bath
- threads
- precipitating bath
- manufacture
- 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
Links
- 229920002678 cellulose Polymers 0.000 title description 20
- 238000004519 manufacturing process Methods 0.000 title description 11
- 229920003086 cellulose ether Polymers 0.000 title description 4
- 230000001376 precipitating effect Effects 0.000 description 36
- 239000000243 solution Substances 0.000 description 18
- 239000001913 cellulose Substances 0.000 description 16
- 238000009987 spinning Methods 0.000 description 16
- 229940081735 acetylcellulose Drugs 0.000 description 15
- 229920002301 cellulose acetate Polymers 0.000 description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- 229920002955 Art silk Polymers 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 230000002522 swelling effect Effects 0.000 description 7
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 6
- SOIFLUNRINLCBN-UHFFFAOYSA-N ammonium thiocyanate Chemical compound [NH4+].[S-]C#N SOIFLUNRINLCBN-UHFFFAOYSA-N 0.000 description 6
- 239000000084 colloidal system Substances 0.000 description 6
- SYUXAJSOZXEFPP-UHFFFAOYSA-N glutin Natural products COc1c(O)cc2OC(=CC(=O)c2c1O)c3ccccc3OC4OC(CO)C(O)C(O)C4O SYUXAJSOZXEFPP-UHFFFAOYSA-N 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- SMEGJBVQLJJKKX-HOTMZDKISA-N [(2R,3S,4S,5R,6R)-5-acetyloxy-3,4,6-trihydroxyoxan-2-yl]methyl acetate Chemical compound CC(=O)OC[C@@H]1[C@H]([C@@H]([C@H]([C@@H](O1)O)OC(=O)C)O)O SMEGJBVQLJJKKX-HOTMZDKISA-N 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 235000013379 molasses Nutrition 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000000578 dry spinning Methods 0.000 description 3
- 238000007654 immersion Methods 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 235000014633 carbohydrates Nutrition 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- 230000003292 diminished effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- -1 monoacetine Chemical compound 0.000 description 2
- 235000018102 proteins Nutrition 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 239000001632 sodium acetate Substances 0.000 description 2
- 235000017281 sodium acetate Nutrition 0.000 description 2
- 238000002166 wet spinning Methods 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- HXDLWJWIAHWIKI-UHFFFAOYSA-N 2-hydroxyethyl acetate Chemical compound CC(=O)OCCO HXDLWJWIAHWIKI-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 229920000715 Mucilage Polymers 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229920000591 gum Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000025 natural resin Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 150000003873 salicylate salts Chemical class 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- BZWKPZBXAMTXNQ-UHFFFAOYSA-N sulfurocyanidic acid Chemical class OS(=O)(=O)C#N BZWKPZBXAMTXNQ-UHFFFAOYSA-N 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 1
- 229960002622 triacetin Drugs 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- 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 a process for the manufacture of artificial threads from a solution of cellulose esters and ethers, according to the wet spinning process, and to the threads obtainable thereby.
- a further object of the present invention is to provide an artificial silk of the class mentioned above, having a dry tensile strength of 2 to 2.5 grams per denier and more.
- Fine threads spun in such a bath by the stretching-spinning process have a tensile strength of about 1.3 to 1.8 grams per denier, which exceeds that of the threads usually obtainable by the dry spinning process to the extent of about 25 to 30%.
- threads are obtainable in which the individual fine fibers are completely separated from one another; after drying, they show an excellent soft feel and an agreeable luster.
- the latter may be modified by varying the spinning conditions by suitable additions to the spinning bath.
- the tensile strength of the threads is essentially increased up to 2.5 grams per denier and more.
- a precipitating bath which contains besides such a salt as retards the coagulation of the threads an organic polymerized substance of high molecular weight, which is colloidly dispersed by water.
- a colloid use, for instance, molasses, sulfite cellulose waste liquor, tanning substances, carbohydrates, such as starch, dextrin, mucilage, gum, or protein-substances, such as gelatin, glue, casein, degraded glutin and the like; furthermore natural resins, soluble synthetic resins, as for instance, the products obtainable from aromatic sulionic acids and aldehydes.
- the quantity of these substances which I add to the precipitating bath may be varied within wide limits.
- the action of the spinning bath may be further modified by adding another salt or other salts which have no or no considerable swelling action upon the substance to be spun, for instance, calcium chloride, magnesium chloride, sodium acetate, ammonium nitrate, or mixtures thereof, or by adding a non-volatile or diflicultly volatile organic substance which has a swelling or dissolving action upon the cellulose product to be spun, for instance, a chlorohydrine, an ester or" a polyvalent alcohol, such as glycol monoacetate, monoacetine, triacetine, an ether of a polyvalent alcohol, such as glycol monomethyl-ether, glycol monoethylether and the like, a monoor polyvalent phenol, a ketone, such as diacetone alcohol, cyclohexanone and its homologues.
- another salt or other salts which have no or no considerable swelling action upon the substance to be spun
- calcium chloride, magnesium chloride, sodium acetate, ammonium nitrate, or mixtures thereof
- the effect of my precipitating bath is not diminished by the fact that a certain amount of the solvent which is used in precipitating the spinning solution is introduced during the spinning process into the precipitating bath, care must be taken, however, that the amount of the solvent present in the precipitating bath does not become too large, and does not exceed about 9%.
- the maximum quantity depends on the quality of the dissolving agent and on the composition of the precipitating bath and will be easily ascertained from time to time by simple experiments. The manufacture of a uniform product on a large scale is, therefore, connected with no difficulties. Recovery of the solvent and the preparation of the precipitating bath is particularly simple if the acetyl cellulose is dissolved in a single solvent, for instance, acetone.
- the length of the threads immersed in the precipitating bath is about 30 cm., but it may be shortened, for example to 15 cm. or extended to 60 cm., or more.
- the threads are then collected on a bobbin or in a spinning centrifuge in the usual manner.
- the threads may be subjected to a stretching procedure in any known manner during. the precipitating step or after their removal from the bath, that is, between the coagulating bath and the collecting device.
- the stretching may be accomplished either by providing a substantial distance between the bath and the collecting device or by leading the threads over rods or rolls arranged in the bath or between the bath and the collecting device.
- the speed of spinning may be varied within wide limits. It depends on the length of immersion of the thread in the precipitating bath, on the opening of the nozzle, on the concentration of the spinning solution, on the quantity of the spinning solution conveyed by the spinning pump to the nozzle, etc.
- the temperature of the precipitating bath and of the spinning solution may also be varied within certain limits, as, for instance, from to 40 C. I prefer to keep them at room temperature, that is to say, at about C.
- Example 1 A solution of 22 per cent. strength of acetyl cellulose in acetone is forced through spinning nozzles having bores of 0.5 mm. diameter into a precipitating bath which contains per liter 200 grams of ammonium sulfocyanide and 550 grams of purified sulfite cellulose waste liquor of specific gravity 1.25.
- the temperature of the bath should be about 20 C. and the length of immersion about 30 centimeters.
- the content of acetone in the bath may vary within wide limits, for example, between 1 and 9 per cent.
- the thread which is spun at a speed of about 15 to 20 meters per minute is washed with water on its way to the spool or to the spinning box.
- a silk is obtained with a nearly circular section, with an individual titer of l to 2 deniers and a dry tensile strength from 2 to 3 grams per denier.
- Example 2 The operation is carried out as described in Example 1, but a precipitating bath is used containing instead of the sulfite cellulose waste liquor per liter 400 grams of molasses residue of specific gravity 1.33.
- molasses residue the final molasses is meant, that is to say, the product which remains after removing the crystallized portions of sugar.
- Example 3 The operation is as described in Example 1, but there are substituted for the sulfite cellulose waste liquor about 500 grams of an aqueous solution of degraded glutin of specific gravity 1.25 per liter of the precipitating bath.
- Example 4 A solution consisting of 20 parts of acetyl cellulose, 2 parts of ammonium sulfocyanide, 4 parts of water and 74 parts of acetone, is spun into a precipitating bath which contains per liter 500 grams of a soluiton of degraded glutin having the specific gravity 1.25 and 40 grams of ammonium sulfocyanide. As mentioned in the preceding examples a silk is obtained with a section approximating to a circular form, the strength of which however is somewhat smaller and amounts to about 2 grams per denier.
- Example 5 A spinning solution consisting of 20 parts of an acetyl cellulose, containing chemically bound 54.5% of acetic acid in 80 parts of acetone is spun into a precipitating bath which contains:
- the temperature of the precipitating bath should be kept at 20, the length of immersion of the thread is about 30 centimeters and the drawing speed about -30 meters per minute. A silk is obtained with nearly circular section, good luster and a dry tensile strength of 2.5 to 3.5 grams per denier.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
- Treatment And Processing Of Natural Fur Or Leather (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE310842T | 1928-05-01 |
Publications (1)
Publication Number | Publication Date |
---|---|
US1997753A true US1997753A (en) | 1935-04-16 |
Family
ID=31894585
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US358762A Expired - Lifetime US1997753A (en) | 1928-05-01 | 1929-04-27 | Manufacture of artificial threads from cellulose esters or cellulose ethers |
Country Status (5)
Country | Link |
---|---|
US (1) | US1997753A (enrdf_load_stackoverflow) |
BE (1) | BE360017A (enrdf_load_stackoverflow) |
FR (1) | FR672962A (enrdf_load_stackoverflow) |
GB (1) | GB310842A (enrdf_load_stackoverflow) |
NL (1) | NL24904C (enrdf_load_stackoverflow) |
-
0
- BE BE360017D patent/BE360017A/xx unknown
- NL NL24904D patent/NL24904C/xx active
-
1929
- 1929-04-11 FR FR672962D patent/FR672962A/fr not_active Expired
- 1929-04-17 GB GB11918/29A patent/GB310842A/en not_active Expired
- 1929-04-27 US US358762A patent/US1997753A/en not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
FR672962A (fr) | 1930-01-09 |
NL24904C (enrdf_load_stackoverflow) | |
BE360017A (enrdf_load_stackoverflow) | |
GB310842A (enrdf_load_stackoverflow) | 1930-07-17 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JPS6366944B2 (enrdf_load_stackoverflow) | ||
US2420949A (en) | Carboxyalkyl cellulose ether fibers and films of good wet strength | |
GB522542A (en) | Improved process for the manufacture of crimped artificial textile filaments, and filaments produced thereby | |
US1997753A (en) | Manufacture of artificial threads from cellulose esters or cellulose ethers | |
US2290789A (en) | Manufacture and production of artificial filaments, threads, and the like | |
US2452130A (en) | Method of spinning high tenacity viscose rayon | |
US2147642A (en) | Production of artificial filaments, films, and like materials | |
GB508781A (en) | Process for the preparation of artificial silk, artificial spun fibres, horsehair, bands, films and the like from phosphoproteins or conjugated proteins | |
US2147641A (en) | Production of artificial filaments, films, and like materials | |
US2145076A (en) | Method of preparing artificial threads | |
US1838121A (en) | Process of preparing artificial textile products with reduced luster from cellulose compounds | |
US2375650A (en) | Manufacture and production of artificial filaments, threads, films, and the like | |
Okajima et al. | Resistance of Valonia cellulose to mercerization | |
US3109699A (en) | Method for making rayon filaments | |
US2122448A (en) | Process for the manufacture of products made from cellulose derivatives | |
US2004273A (en) | Production of cellulose derivative products | |
US2570443A (en) | Method of producing products of animal fibers | |
US2083694A (en) | Manufacture of artificial materials | |
US1920188A (en) | Production of artificial materials | |
US1836254A (en) | Paul xarrer | |
US2671777A (en) | Preparation of organic carboxylic acid esters of cellulose | |
DE610226C (de) | Herstellung von kuenstlichen Gebilden aus Loesungen von Celluloseacetat in organischen Saeuren nach dem Streckspinnverfahren | |
US1949919A (en) | Method of producing artificial threads | |
US1545144A (en) | Method of precipitating artificial threads, ribbons, films, and the like from viscose | |
DE513375C (de) | Verfahren zur Herstellung von Kunstfaeden aus Celluloseestern oder -aethern nach demNassspinnverfahren |