US2762795A - Xanthation - Google Patents

Xanthation Download PDF

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Publication number
US2762795A
US2762795A US274208A US27420852A US2762795A US 2762795 A US2762795 A US 2762795A US 274208 A US274208 A US 274208A US 27420852 A US27420852 A US 27420852A US 2762795 A US2762795 A US 2762795A
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US
United States
Prior art keywords
web
cellulose
carbon
alkali cellulose
chamber
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
Application number
US274208A
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English (en)
Inventor
Schlosser Paul Henry
Mitchell Reid Logan
Robert F Bampton
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rayonier Inc
Original Assignee
Rayonier Inc
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority to BE517038D priority Critical patent/BE517038A/xx
Priority to DENDAT1072353D priority patent/DE1072353B/de
Priority to NL87419D priority patent/NL87419C/xx
Application filed by Rayonier Inc filed Critical Rayonier Inc
Priority to US274208A priority patent/US2762795A/en
Priority to GB32861/52A priority patent/GB734304A/en
Priority to FR1072648D priority patent/FR1072648A/fr
Application granted granted Critical
Publication of US2762795A publication Critical patent/US2762795A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • D01F2/06—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

  • FIG.- 4 XANTHATION Filed Feb. 29. 1952 2 sheets-sheet 2 FIG. 3- y 46 49 45 42 vAcuuM a if ⁇ vAcuuM/ 44 4'7 I 43 @5. FIG.- 4
  • the web of alkali cellulose uniformlyim- ICC pregnated with carbon bisullide may then be led into a heated reaction chamber to effect continuous xanthation of the web while the web is still intact.
  • the carbon bisulfide impregnated web may also be slit into narrow ribbons, broken into fragments or otherwise distntegrated and then charged into a baratte, wet churn or other suitable xanthation reaction vessel.
  • a slitting means such as intermeshing cylindrical shears
  • the alkali cellulose web may be disintegrated by other suitable means such as a breaker of the hammer-mill type, a picker or a continuous shredding device.
  • a breaker of the hammer-mill type such as a picker or a continuous shredding device.
  • Such impregnated and disintegrated alkali cellulose is very suitable for loading into barattes, wet churns, or reactors of the inclined cylindrical cement-mixing type.
  • Alkali cellulose other than in web form may also be conveniently treated with carbon bisulde according to the method of the invention.
  • the slab of alkali cellulose obtained from slurry-type steeping units may be advantageously treated in the manner of the invention.
  • Alkali cellulose of a suitable degree of depolymerization for treating with CS2 on exit from the steeping operation could conveniently be made from a lowviscosity type pulp.
  • several means are also available for making high viscosity cellulose adaptable to such treatment.
  • oxygen could be pulled into the sheet or web of alkali cellulose along with the CS2, thereby accomplishing oxidative degradation and Xanthation in one stage.
  • Metal catalysts such as manganese and cobalt (as described in U. S. 2,542,285 and U. S. application 239,029) could be used to accelerate the alkaline oxidation reaction during xanthation or in a short aging step subsequent to steeping and prior to xanthation.
  • Fig. l is a sectional side view of the apparatus.
  • Fig. 2 is an enlarged fragmentary view at 2-2 of Fig. 1.
  • Figs. l3 and 4 are sectional side views of modifications of apparatus for impregnating moving webs of alkali cellulose with carbon bisulde;
  • Fig. 5 is a sectional side view of apparatus for heating Webs of alkali cellulose afterimpregnation with carbon bisuliide.
  • the apparatus comprises four principal parts, namely, the apparatus A for the impregnation of the web with caustic liquor, the sealed chamber B for the impregnation of the web with carbon bisullide, the chamber C for the removal of excess carbon bisullide, and the chamber Patented Sept. V11, 1956 ⁇ D for retaining the xanthated web under elevated temperatures to complete the reaction.
  • the apparatus A comprises a rotatable perforated drum 1 having. a vacuum section 2 over which the web ofcellulose Apulp 3, comprising two supeiposed sheets. 4.and 5, is passed.
  • Caustic steeping liquor of the type usually used to form alkali cellulose .is sprayed onto the web fromthe supply pipes 6.
  • the vacuum section 2 ismaintained under a reduced pressure by a vacuum pump, not shown, connected to the pipe 7, and the liquor flows through the web in the relative volume as indicated by the shaded area within the curve 9.
  • the impregnated web passes between the perforated drum 1 and the press roller which has a vacuum section 9 embracing the area of contact.
  • the excess caustic liquor is removed from the web by the conjoint action of pressure and vacuum and with a minimum of compacting of the alkali cellulose.
  • the cellulose is not only steeped in a very uniform manner but the excess liquor is effectively and uniformly removed without severely compacting the soft web.
  • the continuously moving web passes between the seal- .ing rollers 12 and 14 and into the sealed chamber B.
  • These rollers are preferably formed of a spongy or otherwise soft rubber which envelop and effectively seal the area of entrance of the web into chamber B.
  • the rotary shears 11 comprise two rollers, each having a multiplicity of round shear blades that slit the web in any desired number of strips. These shear rollers are alternative and may be removed when it is desired not to slit the web. After passing through the shears 11, if used, the two contacting sheets of the webV pass over the spacing bar 18 and are held apart so that liquid carbon bisuliide may be sprayed against the inner opposing faces of the sheets through the perforated pipe 19.
  • rollers Any desired number of such rollers may be used to provide the required number of convolutions or folds of the web to delay its passage sufficiently to permit completion of the xanthation reaction.
  • These rollers may be freely rotatable or power driven by any suitable means (not shown).
  • the web then passes over the guide roller 32 and then between the soft rubber sealing rollers 33 and 34 which are also preferably similar to the sealing rollers 12 and 14.
  • the web of cellulose xanthate, whether in a sheet or longstrips, is dumpedk into a chamber for conversion into viscose.
  • the web in chamber D may be heated in any convenient manner, such as by the infrared heaters 35, which are placed between the folds of the web. Steam coils or resistant heaters may be used for the same purpose.
  • Chambers B and C may be consolidated into a single chamber if desired and operated at any practical pressure. These chambers may be connected to a vacuum pumptnot shown) by the .pipes ,37 andl operated at a pressure slightly belowatmospheric pressure to minimize the escape of carbon bisulfide.
  • the chamber D may also be operated under a slightly reduced pressure by con. necting the pipe 38 to a vacuum pump.
  • the carbon bi sulde removed from chambers B, C and D and the vacuum members 25 and 26 may be pumped through a xanthation chamber for the absorption of the carbon bisullide vapors in a batch of liuffy alkali cellulose, or it may be recovered in an activated carbon absorption unit and returned to the process.
  • the chambers B, C and D are sealed only to exclude or retain gases under a very slight pressure difference.
  • the sealing may not be absolute since we contemplate a certain amount of permissible leakage as by allowing some air to seep in around the rollers to prevent an escape of carbon bisulfide.
  • the apparatus of Fig. 3 comprises a single enclosed chamber B--C with sealing rollers 40-41 at the end where the web of alkali cellulose 3 enters and sealing rollers 42--43 where the web leaves.
  • the two sheets 4 and 5 are separated and treated with carbon bisulde as in Fig. l.
  • the web. is supported from below by the endless screen .44 which travels as a belt, and may be slit into strips by passing through the rotary shears 45.
  • the excess carbon bisulfide is pulled through the sheets by thevacuum members 46-47.
  • Member 46 is directly over the endless.
  • screen 49 and member 47 is directly under screen 44 and the web is accordingly supported on both sides while under vacuum.
  • the entire chamber B-C ⁇ may be. operated Yunder sub-atmospheric pressure by connecting the pipe 50 to a vacuum pump.
  • Fig. 4 The apparatus of Fig. 4 comprises a single enclosed chamber B-C, sealing rollers 40-41, 42-43, vacuum pump 50, endless screen 44 and vacuum member 47 as in Fig. 4.
  • the web 3 of alkali cellulose consisting of sheets4 and 5 passes under the perforated pipe 52 and is showered with carbon bisulfide just in advance of the vacuumkmember. The carbon bisulflde is pulled through the web by the vacuum, the excess enteringthe vacuum system.
  • Fig. 5 illustrates a modified treating chamber D having sealing rollers at the web entering and exiting ends and a pipe 51 for operatingthe chamber under a rcduced pressure.
  • this chamber D is operated in combination with a chamber B-C of Fig. 3 or 4, the sealingrollersy 42-43 and end wall can form the entering sealing rollers and wall of chamber D.
  • the web 3 which had been impregnated with carbon bisulde as in Figs.I l, 2 and 3, passes between electronic heating devices 52.
  • the invention very materially increases the efficiency of xanthation due to several factors.
  • the alkali cellulose is relatively free of excess alkali and is in a relatively loose or porous state in contrast to the compacted mass of alkali cellulose usually resultingjfrom ⁇ compression to squeeze out the excess caustic.
  • the xanthation is very efficient and can be carried lout in a shorter time on a much less bulky material than the shredded alkali cellulose and with at least equal effectiveness. It eliminates the rcumbersome and bulky equipment now necessary.

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  • 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)
  • Nonwoven Fabrics (AREA)
  • Paper (AREA)
US274208A 1952-02-29 1952-02-29 Xanthation Expired - Lifetime US2762795A (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
BE517038D BE517038A (en(2012)) 1952-02-29
DENDAT1072353D DE1072353B (en(2012)) 1952-02-29
NL87419D NL87419C (en(2012)) 1952-02-29
US274208A US2762795A (en) 1952-02-29 1952-02-29 Xanthation
GB32861/52A GB734304A (en) 1952-02-29 1952-12-29 Improvements in xanthation of cellulose
FR1072648D FR1072648A (fr) 1952-02-29 1953-01-16 Xanthation de la cellulose

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US274208A US2762795A (en) 1952-02-29 1952-02-29 Xanthation

Publications (1)

Publication Number Publication Date
US2762795A true US2762795A (en) 1956-09-11

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Application Number Title Priority Date Filing Date
US274208A Expired - Lifetime US2762795A (en) 1952-02-29 1952-02-29 Xanthation

Country Status (6)

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US (1) US2762795A (en(2012))
BE (1) BE517038A (en(2012))
DE (1) DE1072353B (en(2012))
FR (1) FR1072648A (en(2012))
GB (1) GB734304A (en(2012))
NL (1) NL87419C (en(2012))

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4158698A (en) * 1975-09-04 1979-06-19 Fiber Associates, Inc. Apparatus for continuous xanthation and production of viscose spinning solution

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US520770A (en) * 1894-06-05 Plastic compound of cellulose
US765508A (en) * 1903-12-19 1904-07-19 Lewis W Noyes Machine for coating paper or like materials.
US1672249A (en) * 1927-06-27 1928-06-05 George H Ellis Apparatus for making composition boards or sheets
US1884486A (en) * 1928-12-19 1932-10-25 Barrett Co Impregnating process
US1892579A (en) * 1931-04-16 1932-12-27 Kilner Arthur Hugoe Apparatus for the production and manufacture of material impregnated with cellulose regenerated from viscose or other cellulosic solutions
US2011156A (en) * 1933-07-19 1935-08-13 Nelson Harry Huet Process for the manufacture of paper
US2092306A (en) * 1934-08-13 1937-09-07 Marbo Patents Inc Apparatus for reacting organic web materials with liquefied reagents
US2122519A (en) * 1935-10-02 1938-07-05 American Enka Corp Manufacture of artificial silk
US2126044A (en) * 1932-05-19 1938-08-09 Int Paper Co Manufacture of soluble cellulose
US2384298A (en) * 1941-09-19 1945-09-04 Jasco Inc Apparatus for the manufacture of high molecular weight polymers
US2530403A (en) * 1946-11-21 1950-11-21 Stewart E Seaman Continuous xanthation

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US520770A (en) * 1894-06-05 Plastic compound of cellulose
US765508A (en) * 1903-12-19 1904-07-19 Lewis W Noyes Machine for coating paper or like materials.
US1672249A (en) * 1927-06-27 1928-06-05 George H Ellis Apparatus for making composition boards or sheets
US1884486A (en) * 1928-12-19 1932-10-25 Barrett Co Impregnating process
US1892579A (en) * 1931-04-16 1932-12-27 Kilner Arthur Hugoe Apparatus for the production and manufacture of material impregnated with cellulose regenerated from viscose or other cellulosic solutions
US2126044A (en) * 1932-05-19 1938-08-09 Int Paper Co Manufacture of soluble cellulose
US2011156A (en) * 1933-07-19 1935-08-13 Nelson Harry Huet Process for the manufacture of paper
US2092306A (en) * 1934-08-13 1937-09-07 Marbo Patents Inc Apparatus for reacting organic web materials with liquefied reagents
US2122519A (en) * 1935-10-02 1938-07-05 American Enka Corp Manufacture of artificial silk
US2384298A (en) * 1941-09-19 1945-09-04 Jasco Inc Apparatus for the manufacture of high molecular weight polymers
US2530403A (en) * 1946-11-21 1950-11-21 Stewart E Seaman Continuous xanthation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4158698A (en) * 1975-09-04 1979-06-19 Fiber Associates, Inc. Apparatus for continuous xanthation and production of viscose spinning solution

Also Published As

Publication number Publication date
FR1072648A (fr) 1954-09-14
NL87419C (en(2012))
GB734304A (en) 1955-07-27
BE517038A (en(2012))
DE1072353B (en(2012)) 1959-12-31

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