US2139302A - Manufacture of viscose - Google Patents
Manufacture of viscose Download PDFInfo
- Publication number
- US2139302A US2139302A US170292A US17029237A US2139302A US 2139302 A US2139302 A US 2139302A US 170292 A US170292 A US 170292A US 17029237 A US17029237 A US 17029237A US 2139302 A US2139302 A US 2139302A
- Authority
- US
- United States
- Prior art keywords
- viscose
- alkali cellulose
- viscosity
- air
- 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
- 229920000297 Rayon Polymers 0.000 title description 20
- 238000004519 manufacturing process Methods 0.000 title description 5
- 229920002678 cellulose Polymers 0.000 description 28
- 239000001913 cellulose Substances 0.000 description 28
- 239000003513 alkali Substances 0.000 description 22
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 18
- 238000000034 method Methods 0.000 description 12
- 230000032683 aging Effects 0.000 description 11
- 238000009987 spinning Methods 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- ZOOODBUHSVUZEM-UHFFFAOYSA-N ethoxymethanedithioic acid Chemical compound CCOC(S)=S ZOOODBUHSVUZEM-UHFFFAOYSA-N 0.000 description 6
- 239000012991 xanthate Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000007664 blowing Methods 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 3
- 239000003518 caustics Substances 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920002955 Art silk Polymers 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005499 meniscus Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010517 secondary reaction Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 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
Definitions
- This invention relates to the manufacture of viscose artificial silk and more particularly to a novel method of controlling and regulating the viscosity of viscose spinning solutions.
- the alkali cellulose During the conventional processing steps to convert cellulosic material into spinning solutions of the viscose type, the alkali cellulose must be suitably aged in order to provide a spinning solution having the proper viscosity for practical working operations. If the aging step be omitted, then the viscosity of the viscose solution is too high. It is well known that the degree of aging is dependent on several factors, e. g., aging temperature, aging time and the amount of oxygen coming in contact with the alkali cellulose. If the air containing oxygen is prevented from contacting the alkali cellulose, substantially no aging occurs, or at least, it occurs much more slowly.
- Still another proposal to reduce the viscosity contemplates the contacting of alkali cellulose with a gas that is richer in oxygen content than is the atmosphere. This method also has objections and is far from economical.
- the object of the present invention to provide a method whereby the aging of the alkali cellulose can be entirely eliminated or, at least, theaging period shortened considerably.
- a further object contemplates a relatively simple process that can be practiced without the use of any special chemicals and at normal temperacifically.
- the normal xanthating operation is interrupted after only a portion of the usual quantity of carbon disulphide has been added.
- this definite amount of carbon disulphide has been absorbed by the alkali cellulose crumbs,
- the sulphurizing zone for a short period.
- the remaining quantity of carbon disulphide necessary to fully react with the alkali cellulose is added in the normal way and the resulting cellulose Xanthate is dissolved in dilute alkali to form viscose.
- the decrease in viscosity of the viscose according to this method is much greater than when the same amount of air contacts with entirely undesulphurized alkali cellulose or with normally finished xanthate, the temperature being. maintained the same in all cases.
- the decrease in viscosity of the spinning solution passes through a sharply defined maximum.
- the maximum decrease in viscosity is obtained when the quantity of carbon disulphide added before introducing the air is between 60. and of the total quantity needed.
- the tables set forth below indicate the results of several experiments. These results were obtained when using an alkali cellulose without aging and having a composition comprising 15.5% sodium hydroxide and 29% cellulose and other innocuous constituents.
- the figures which indicate the final viscosity of the viscose are expressed in seconds and are determined by means of a tube-viscosimeter. This viscosimeter consists of a vertical glass-tube of 5.2 mm. internal diameter, open at both ends and which possesses two marks at a distance of 230 mm. The tube is filled with viscose, which is then allowed to flow out under the influence of its own hydrostatic pressure.
- a preparatory treatment for the manufacture of viscose having a normal viscosity from unaged alkali cellulose which comprises forming alkali cellulose and immediately partially sulphurizing the same, suspending the sulphurizing step and introducing air into the alkaline sulphurizing zone and finally completing the sulphurizing action on the alkali cellulose to produce cellulose xanthate.
- a method of converting unaged alkalicellulose into viscose having a normal viscosity which comprises incompletely xanthating alkali cellulose immediately after it has been formed, contacting air containing oxygen with the partially reacted alkaline mass for a limited period, completing the xanthating operation and dissolving the cellulose xanthate in a dilute caustic solution to produce viscose.
- a method according to claim 2 which further provides for the addition of 60 to of the total amount of carbon disulphide needed prior to the introduction of air.
- a method of converting unaged alkali cellulose into viscose having a normal viscosity which comprises partially xanthating alkali cellulose by reacting 25% carbon disulphide, based on the weight of dry cellulose in the alkali cellulose, with alkali cellulose, blowing air containing oxygen in the xanthating zone for at least two hours, completing the xanthating operation by the further addition of 12% carbon disulphide based on the weight of dry cellulose in the alkali cellulose and dissolving the thus formed cellulose xanthate in a dilute caustic solution to produce viscose.
- a method according to claim 2 which further provides for contacting air with the partially reacted mass for a period from three to four hours at a temperature of approximately 25 C.
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Artificial Filaments (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
NL2139302X | 1936-10-23 |
Publications (1)
Publication Number | Publication Date |
---|---|
US2139302A true US2139302A (en) | 1938-12-06 |
Family
ID=19873725
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US170292A Expired - Lifetime US2139302A (en) | 1936-10-23 | 1937-10-21 | Manufacture of viscose |
Country Status (3)
Country | Link |
---|---|
US (1) | US2139302A (en:Method) |
DE (1) | DE719691C (en:Method) |
NL (1) | NL43454C (en:Method) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2520963A (en) * | 1947-06-06 | 1950-09-05 | Richard E Reeves | Production of improved cellulosic materials |
US2560391A (en) * | 1947-03-24 | 1951-07-10 | Lenzinger Zellwolle Und Papier | Process for treating of cellulose material |
US2647114A (en) * | 1949-05-07 | 1953-07-28 | Phrix Werke Ag | Method for making readily filterable viscose |
US2985647A (en) * | 1959-01-12 | 1961-05-23 | Kohorn Oscar Von | Manufacture of viscose spinning solution |
US4076934A (en) * | 1976-10-22 | 1978-02-28 | Olin Corporation | Method for controlling oxygen level during continuous xanthation of alkali cellulose |
-
0
- NL NL43454D patent/NL43454C/xx active
-
1937
- 1937-09-30 DE DEN41199D patent/DE719691C/de not_active Expired
- 1937-10-21 US US170292A patent/US2139302A/en not_active Expired - Lifetime
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2560391A (en) * | 1947-03-24 | 1951-07-10 | Lenzinger Zellwolle Und Papier | Process for treating of cellulose material |
US2520963A (en) * | 1947-06-06 | 1950-09-05 | Richard E Reeves | Production of improved cellulosic materials |
US2647114A (en) * | 1949-05-07 | 1953-07-28 | Phrix Werke Ag | Method for making readily filterable viscose |
US2985647A (en) * | 1959-01-12 | 1961-05-23 | Kohorn Oscar Von | Manufacture of viscose spinning solution |
US4076934A (en) * | 1976-10-22 | 1978-02-28 | Olin Corporation | Method for controlling oxygen level during continuous xanthation of alkali cellulose |
Also Published As
Publication number | Publication date |
---|---|
NL43454C (en:Method) | |
DE719691C (de) | 1942-04-18 |
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