Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
  • C08L1/02—Cellulose; Modified cellulose
  • C08L1/06—Cellulose hydrate
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
  • C08B16/00—Regeneration of cellulose
• • 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

• the invention relates to a method of preparation of staple fibers and filaments of high wet and dry strength as well as excellent knot strength. That is, the fibers produced in accordance with the present invention are highly resistant to stresses exerted in the direction of the fiber axis as Well as to any stress which may be exerted perpendicular to the fiber axis.
• the process of this invention comprises producing alkali cellulose of a relatively high degree of polymerization and of uniform structure, that is, distribution of degree of polymerization is uniform, and of the three steps for preparing viscose from such alkali cellulose: to wit, the first step of adding (MS-0.3% of an alkylene oxide polymer, or an adduct of amine and alkylene oxide, or an acid amide, to the solution of the xanthate prepared from the alkali cellulose as described; the second step o coagulating the viscose in a spinning bath containing 0.005-0.3% of a divalent metallic salt; and the third step of regenerating the as-spun filaments having a suitable degree of regeneration through the second bath.
• pulp be utilized having an average degree of polymerization of 1200 or more.
• alkali cellulose of high degree of ploymerization and of very even distribution of polymerization can be obtained.
• alkali cellulose is xanthated with, say, more than 40%, preferably 40-70%, of carbon disulfide, because of the even distribution of degree of ploymerization of the alkali cellulose, very well xanthated viscose which is easily soluble in alkali of lower concentration than is required for conventional xanthate or in pure water and furthermore which has good dispersion property is obtained.
• the gist of this invention lies, in addition to such process for production of viscose, in the concept of adding such substances as polyalkyleue oxide, acid amide, adduct of amine and alkylene oxide, etc. to the dissolving solution at the viscose-dissolving step, making viscose and Spinning the same.
• these substances generally possess surface active properties, they serve to better the dispersion state of xanthate in the alkali solution. Furthermore because they greatly influence, together with byproducts in the viscose, permeation and diffusion of hydrogen ion and divalent metallic ion to the filaments at the time of spinning of the viscose, it is possible to optionally adjust the state of coagulation and regeneration of the viscose flow by varying the amount of addition of these substances.
• the process of the present invention makes such controls possible for an industrial process for the first time. Moreover, optimum results with said viscose can be obtained by spinning the same in a spinning bath containing at least 0.005% but not more than 0.3% of a divalent metallic salt.
• the amount of addition must of course be fitted to the temperature of the spinning bath. At such a low concentration as close to 0.005%, a relatively low temperature should be employed, whereas at a high concentration of about 0.3%, a high temperature of above 40 C. is required. This is why the temperature of the spinning bath should be within the specified range of 20-45 C.
• Still another critical feature of the present invention is the use of a second bath in addition to the first bath described above. That is, even under the optimum conditions for production of the viscose and of the spinning bath, without the use of a second bath, the achievements as of this invention cannot be expected.
• the second bath has been provided only for the purpose of aiding the regeneration of filaments, and no particular care has been taken for the formation process of the filaments in the second bath.
• pulp of an average degree of polymerization of, preferably 1200 or more is steeped in alkali, shredded, and aged for at least 10 hours at below 20 C., to yield an alkali cellulose of high average degree of polymerization and further of even distribution of polymerization.
• Said alkali cellulose is xanthated with, for example, 40% or more of carbon disulfide, and the resultant good xanthate is dissolved in diluted caustic soda solution or pure water containing additives listed below, to make a viscose containing 48% of cellulose, 3-6% of alkali, and 0.15-0.3% of the additives.
• the additives useful in the present invention are as follows: polyalkylene om'de, acid amide, and adduct of amine and alkylene oxide.
• polyalkylene oxide those of general formula wherein:
• R and R are selected from the group consisting of hydrogen, alkyl or aryl groups having more than 4 but not more than 10 carbon atoms, and may be same or different,
• n is a positive integer of 2-10 and m is a positive integer of 5-100 are used.
• alkylene oxide polymer it may be a polymethylene oxide polymer having the formula:
• the acid amide may be represented by the formula 'RCONH wherein R is an alkyl or alkyl group of 1-18 carbon atoms.
• amine-alkylene oxide adduct those having the following formula may be used:
• R and R are selected from the group consisting of hydrogen, alkyl, or aryl groups having more than 4 but not more than 10 carbon atoms, and may be same or different,
• n is a positive integer of 2-10
• x+y is a positive integer of 5-100, preferably 5-20.
• composition of the coagulation bath must be such that the bath contains not more than 5% of sulfuric acid, not more than 15% of sodium sulfate, and 0.005-0.3% of a divalent metallic salt, such as divalent sulfate of Zn, Ni, Co, Cd, and Cr.
• a divalent metallic salt such as divalent sulfate of Zn, Ni, Co, Cd, and Cr.
• the filaments of which regeneration value before entering into the second bath is adjusted to 4060% are passed through the second bath of a temperature above C. containing not more than 1.5% of sulfuric acid and wound up with tension.
• a monophenol ether of polyalkylene glycol i.e., a monophenol ether of polyalkylene glycol
• the properties of the fiber so obtained was as shown as A in Table I.
• B is that whose other processing steps were completely identical to that of the process of this invention, but in which the viscose preparation process the material pulp used was that having a degree of polymerization of about 800, aging was not performed and the degree of polymerization of the product was made to be about the same as that according to the present invention.
• C in the table is that in which the viscose preparation process was completely identical to the process of this invention, but in which an additive was not incorporated during dissolving.
• D is that in which the viscose preparation step was identical to that of this invention, but in which the spinning bath did not contain a divalent metallic salt.
• a process for the preparation of regenerated cellulose fibers from viscose comprising producing cellulose xanthate from an alkali cellulose having a relatively high degree and even distribution of polymerization which has been obtained by using pulp having an average degree of polymerization of not less than 1200, adding and dissolving in the cellulose xanthate an additive selected from the group consisting of an alkylene oxide polymer, an adduct of an amine with an alkylene oxide, and an acid amide to make a viscose, said additive being added in such proportion that the viscose contains 0.15 to 0.30 percent of the same, spinning said viscose at a temperature of C. to 45 C.
• a first spinning bath containing 0.0050.3 percent of a divalent metallic salt, thereafter subjecting the resultant filaments having a regeneration value of -60 percent to tension in a second bath having a temperature of at least C. and a sulfuric acid concentration of not more than 1.5 percent.
• alkali cellulose is obtained by a process which consists of steeping pulp having an average degree of polymerization of not less than 1200 in alkali, shredding the resultant alkali cellulose, and thereafter aging the same for ten to 20 hours at a temperature not higher than about 20 C.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Engineering & Computer Science (AREA)
• Medicinal Chemistry (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Health & Medical Sciences (AREA)
• Life Sciences & Earth Sciences (AREA)
• Biochemistry (AREA)
• Materials Engineering (AREA)
• General Chemical & Material Sciences (AREA)
• Textile Engineering (AREA)
• Artificial Filaments (AREA)

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Cited By (3)

Citations (10)

• 0
  • BE BE632898D patent/BE632898A/xx unknown
  • NL NL293298D patent/NL293298A/xx unknown
• 1963
  • 1963-05-27 ES ES288427A patent/ES288427A1/es not_active Expired
  • 1963-05-27 US US283540A patent/US3381075A/en not_active Expired - Lifetime
  • 1963-05-28 DE DE19631494745 patent/DE1494745A1/de active Pending
  • 1963-05-28 GB GB21312/63A patent/GB1029736A/en not_active Expired
  • 1963-05-28 AT AT429963A patent/AT255019B/de active
  • 1963-05-28 CH CH665763A patent/CH451398A/de unknown

Patent Citations (10)

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