US2898222A - Manufacture of regenerated cellulose - Google Patents
Manufacture of regenerated cellulose Download PDFInfo
- Publication number
- US2898222A US2898222A US562352A US56235256A US2898222A US 2898222 A US2898222 A US 2898222A US 562352 A US562352 A US 562352A US 56235256 A US56235256 A US 56235256A US 2898222 A US2898222 A US 2898222A
- Authority
- US
- United States
- Prior art keywords
- viscose
- cellulose
- manufacture
- ethylene oxide
- regenerated cellulose
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000004627 regenerated cellulose Substances 0.000 title claims description 6
- 229920000297 Rayon Polymers 0.000 claims description 26
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical class C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 13
- 150000003141 primary amines Chemical class 0.000 claims 1
- 229920002678 cellulose Polymers 0.000 description 12
- 239000001913 cellulose Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000654 additive Substances 0.000 description 9
- 230000000996 additive effect Effects 0.000 description 8
- 125000001931 aliphatic group Chemical group 0.000 description 8
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 5
- 238000009987 spinning Methods 0.000 description 5
- 239000012991 xanthate Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 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 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229920000298 Cellophane Polymers 0.000 description 1
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- -1 ethenoxy Chemical group 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 235000015250 liver sausages Nutrition 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 235000013580 sausages Nutrition 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 235000009529 zinc sulphate Nutrition 0.000 description 1
- 239000011686 zinc sulphate 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
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
- D01F2/10—Addition to the spinning solution or spinning bath of substances which exert their effect equally well in either
Definitions
- This invention relates to new and useful improvements in the manufacture of regenerated cellulose from viscose into such articles as continuous filament tire yarn, textile yarn staple fibre, cellophane or sausage casings and the like, and particularly seems to provide a novel process in which the physical characteristics of the articles -produced thereby are markedly superior .to those obtained through the practice of previous processes.
- cellulose In the production of viscose threads, cellulose, usually in the form of highly-refined dissolving wood pulp, is converted into alkali cellulose by treatment with caustic soda solution. The alkali cellulose so formed, after ageing, is converted into sodium cellulose xanthate by reaction with carbon disulphide. The sodium cellulose xanthate is dissolved in weak caustic soda solution to form the viscose solution. The viscose is then filtered, aged, and extruded through fine holes of a spinnerette into a spinning bath which normally consists of sulphuric acid and salts such as sodium sulphate and zinc sulphate.
- the filaments thus formed are stretched in a plasticizing bath and are then treated with purifying solution, which in some cases may simply be hot water, and then are treated with a finish or sizing solution, and then are dried and wound into suitable packages.
- purifying solution which in some cases may simply be hot water
- n is an integer between 4 and 50.
- Benefits will be conferred by 4 to 50 ethylene oxide units in the ethenoxy portion of these amide condensation products, but best results are obtained with to 30 ethylene oxide units.
- the additive was "Priminox 32 where n, the number of moles of ethylene oxidein'the molecule, was-equalrto 25. .Acomparative untreated batch .of viscose .was :also made rand spun under identical conditions to the batches containing the additives.
- Viscosity ball fall 60-70 poises. Spinning speed 50 metres/minute. Denier 1'650'(72O'filaments). Immersion of acid bath '28 inches.
- the products may be added at almost any stage of the viscose process and even to the raw material cellulose itself if desired.
- addition to the mixing solution the weak caustic soda solution used to dissolve the xanthate
- dissolution of the xanthate therein is the simplest and most eificient method.
- n is an integer between 10 and 30.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Artificial Filaments (AREA)
Description
rates Pate MANUFACTURE .OF REGENERATED CELLULOSE No Drawing. Application January 30, "1956 Serial No."562,352
l Clairns. (Cl. 106-465) This invention relates to new and useful improvements in the manufacture of regenerated cellulose from viscose into such articles as continuous filament tire yarn, textile yarn staple fibre, cellophane or sausage casings and the like, and particularly seems to provide a novel process in which the physical characteristics of the articles -produced thereby are markedly superior .to those obtained through the practice of previous processes.
In the production of viscose threads, cellulose, usually in the form of highly-refined dissolving wood pulp, is converted into alkali cellulose by treatment with caustic soda solution. The alkali cellulose so formed, after ageing, is converted into sodium cellulose xanthate by reaction with carbon disulphide. The sodium cellulose xanthate is dissolved in weak caustic soda solution to form the viscose solution. The viscose is then filtered, aged, and extruded through fine holes of a spinnerette into a spinning bath which normally consists of sulphuric acid and salts such as sodium sulphate and zinc sulphate. In the production of viscose threads for tire yarn the filaments thus formed are stretched in a plasticizing bath and are then treated with purifying solution, which in some cases may simply be hot water, and then are treated with a finish or sizing solution, and then are dried and wound into suitable packages.
We have now found that, under certain conditions of coagulation and regeneration of the viscose filaments in the spinning bath, a substantial difference in cross-sections and marked improvement in the physical properties of the yarn so formed can be achieved if there is present in the viscose in suflicient quantity one or more derivatives of ethylene oxide and aliphatic tertiary-alkyl primary amines. Such products have the generic formula:
where n is an integer between 4 and 50.
One such product which has been found satisfactory in the practice of this invention is Priminox as presently manufactured by Rohm & Haas Co.
Benefits will be conferred by 4 to 50 ethylene oxide units in the ethenoxy portion of these amide condensation products, but best results are obtained with to 30 ethylene oxide units.
In accomplishing the objects of this invention we have found that it is necessary to incorporate in the viscose at least 1% by weight on the cellulose content of the viscose, and preferably 2% should be used. No further advantage can be obtained by using more than 4%.
The following examples will illustrate preferred embodiments of this invention, but the invention must not be construed as limited solely to these examples:
EXAMPLE 1 Two percent, by weight based on the cellulose content of the viscose (oven dry basis), of derivatives of ethylene oxide and aliphatic tertiary-alkyl primary amines known commercially under the trademark Priminox were added to viscoses and spun "into tire yarnunder the conditions given below. In each .caseaddition was made to the mixing solution before the .xanthate was dissolved therein. where n, the number :of moles .of ethylene :oxide :in the In one lease the additive *was fPriminox =43" molecule, was equal to 1. In another case the additive was "Priminox 32 where n, the number of moles of ethylene oxidein'the molecule, was-equalrto 25. .Acomparative untreated batch .of viscose .was :also made rand spun under identical conditions to the batches containing the additives.
Spinning conditions: Viscose composition 7% cellulose-6% .{NaQ Ripening index, Hottenroth v30.
'Ripening-index, salt vtest 510.0.
Viscosity, ball fall 60-70 poises. Spinning speed 50 metres/minute. Denier 1'650'(72O'filaments). Immersion of acid bath '28 inches.
Temperature .of acid tbath 60 :C. Acid bath.composition H2804 g./l. ZnSO 122.7 g./l. Density, 20 C 1.274.
Percent stretch in second bath The yarn so produced as twisted into a 2 ply cord of It can be seen that the batch containing the additive Priminox 43 where the number of moles of ethylene oxide in the additive molecule was only one, was actually inferior in cord properties to the control batch containing no additive whereas the batch containing the additive Priminox 32 where the number of moles of 'ethylene oxide in the additive molecule was 25 gave cord properties markedly superior to the control batch containing no additive. Furthermore, the cross-sections of the yarn produced from the batch containing Priminox 32 were markedly different from those produced from the control batch.
The products may be added at almost any stage of the viscose process and even to the raw material cellulose itself if desired. However, for the accomplished purpose of the object of this invention we have found that addition to the mixing solution (the weak caustic soda solution used to dissolve the xanthate) before dissolution of the xanthate therein is the simplest and most eificient method.
Many variations of this process will suggest themselves .to those skilled in the art, but such variations are considered as falling within the scope of this invention, provided the products employed are within the class described.
We claim:
1. In the manufacture of regenerated cellulose by the viscose process, the step of incorporating in the viscose from about 1% to about 4%, based on the weight of celluose in the viscose, of derivatives of ethylene oxide 3 and aliphatic tertiary-alkyl primary amines having the generic formula where n is an integer between 4 and 50.
2. The method of claim 1 in which the amount of derivatives of ethylene oxide and aliphatic tertiary-alkyl primary amines is about 1% based on the cellulose in the viscose.
3. The method of claim 1 in which the amount of derivatives of ethylene oxide and aliphatic tertiary-alkyl primary amines is about 2% based on the cellulose in the viscose.
4. The method of claim 1 in which n is 25.
5. In the manufacture of regenerated cellulose by the viscose process, the step of spinning viscose in the presence of from about 1% to about 4%, based on the weight of cellulose in viscose, of derivatives of ethylene oxide and aliphatic tertiary-alkyl primary amines having the generic formula where n is an integer between 4 and 50.
6. The method of claim 5 in which the amount of derivatives of ethylene oxide and aliphatic tertiary-alkyl where n is an integer between 4 and 50.
9. The method of claim 5 in which the amount of derivatives of ethylene oxide and aliphatic tertiary-alkyl primary amines is about 2% based on cellulose in viscose and in which n is 25.
10. The method of claim 1 in which n is an integer between 10 and 30.
References Cited in the file of this patent UNITED STATES PATENTS 2,535,044 Cox Dec. 26, 1950 2,593,466 MacLaurin et a1. Apr. 22, 1952 2,710,861 Charles et a]. June 14, 1955
Claims (1)
1. IN THE MANUFACTURE OF REGENERATED CELLULOSE BY THE VISCOSE PROCESS, THE STEPS OF INCORPORATING IN THE VISCOSE FROM ABOUT 1% TO ABOUT 4%, BASED ON THE WEIGHT OF CELLUOSE IN THE VISCOSE, OF DERIVATIVES OF ETHYLENE OXIDE AND ALIPHATIC TERTIARY-ALKYL PRIMARY AMINES HAVING THE GENERIC FORMULA
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US562352A US2898222A (en) | 1956-01-30 | 1956-01-30 | Manufacture of regenerated cellulose |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US562352A US2898222A (en) | 1956-01-30 | 1956-01-30 | Manufacture of regenerated cellulose |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2898222A true US2898222A (en) | 1959-08-04 |
Family
ID=24245930
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US562352A Expired - Lifetime US2898222A (en) | 1956-01-30 | 1956-01-30 | Manufacture of regenerated cellulose |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2898222A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2535044A (en) * | 1947-04-26 | 1950-12-26 | Du Pont | Spinning of viscose |
| US2593466A (en) * | 1948-07-16 | 1952-04-22 | Ind Rayon Corp | Viscose spinning solution |
| US2710861A (en) * | 1951-08-20 | 1955-06-14 | Int Paper Canada | Treatment of cellulose with the reaction product of primary aliphatic amines and ethylene oxide |
-
1956
- 1956-01-30 US US562352A patent/US2898222A/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2535044A (en) * | 1947-04-26 | 1950-12-26 | Du Pont | Spinning of viscose |
| US2593466A (en) * | 1948-07-16 | 1952-04-22 | Ind Rayon Corp | Viscose spinning solution |
| US2710861A (en) * | 1951-08-20 | 1955-06-14 | Int Paper Canada | Treatment of cellulose with the reaction product of primary aliphatic amines and ethylene oxide |
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