Classifications

• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
  • C08K5/00—Use of organic ingredients
  • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
  • C08K5/0041—Optical brightening agents, organic pigments
• • 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
  • D01F2/16—Addition of dyes to the spinning solution

Definitions

• the brightener should at most be only sparingly soluble in water to avoid a solution of the brightener in the coagulating bath. On the other hand, it must be possible to dissolve the brightener in the emulsifiers to be used, if necessary with the aid of a suitable solution promoter.
• the emulsifiers used are nonionic substances, especially polyglycol condensation products with higher alcohols and with para-alkyl phenols containing higher alkyl radicals or reaction products of long chain fatty acids with substituted amines.
• This invention relates to a process for the manufacture of optically brightened shaped articles from regenerated cellulose treated with organic, water-insoluble brightening agents.
• Shaped products can be optically brightened during their manufacture by one of two fundamentally different methods: During the finishing of the material it may be treated in an after-treating bath, especially in the scrooping bath, with a water-soluble brightening agent which deposits on the material from these baths more or less rapidly, or the optical brightener may be incorporated with the mass from which the product is shaped.
• optical brighteners may be particularly objectionable in scrooping baths since the latter are used for various products, including those which are not intended to be brightened.
• the brightener in the scrooping bath attains in the course of time a concentration that may cause patchy brightening effects.
• the second method referred to above that is to say the incorporation of finely dispersed water-insoluble brighteners with the viscose rayon spinning mass, produces as a rule no brightening effects or only minor ones and, in addition, in many cases the brighteners own color causes yellowing of the material under treatment.
• the present invention provides a process in which the brightener is added to the viscose rayon mass as described for the second method referred to above, but it produces good brightening effects that are fast to washing.
• a solution of an optical brightener in an emulsifier is added to the viscose spinning mass before its coagulation and shaping.
• regenerated cellulose refers to material obtained from natural cellulose by alkalinization, sulfidation and shaping in a coagilating bath, with the viscose rayon obtained by sulfidation and dissolution being made up, for example, in tows, foils or tapes or preferably fibers. Either continuous or staple fibers may be produced.
• optical brighteners to be used in the present process may belong to a wide variety of chemical compounds. Inter alia, for example, there may be used dib nzoxazolylthiophenes, 4,4 di-triazinylaminostilbene-Z,2'-disulfonic acids further substituted on the triazine rings, coumarins or 1,4-distyrylbenzenes.
• the brightener should at most be only sparingly soluble in water so that the coagulating or scrooping bath will not dissolve an appreciable amount of the brightener concerned.
• the above-mentioned 4,4 di-triazinylaminostilbene-2,2'-disulfonic acids should contain no further groups imparting solubility in water.
• emulsifiers that is to say, quite generally speaking, surface-active substances. It is of advantage to use as such substances nonionic emulsifiers, especially polyglycol compounds containing a higher aliphatic hydrocarbon residue.
• nonionic emulsifiers especially polyglycol compounds containing a higher aliphatic hydrocarbon residue.
• a large variety of such products is known; they are obtained, for example, by an additive reaction of ethylene oxide with higher alcohols, with para-alkylphenols containing higher alkyl radicals or with higher alkylmercaptans.
• Suitable products are the reaction products of fatty acids of higher molecular weight with hydroxyalkylamines such as triethanolamine and more especially diethanolamine which may be reacted with ethylene oxide.
• an organic solvent which may be miscible with water in all proportions, as is the case e.g. with dioxane, or it may be only restrictedly water-miscible, for example to an extent up to percent, as is the case with butanol or cyclohexane. It is also of great advantage to add a higher fatty acid, such as oleic, stearic, palmitic or lauric acid, or a salt thereof.
• optical brightener is dissolved in an organic solvent which is readily miscible with water (preferably in all proportions), such as dioxane, glycol monobutyl ether or propanol, and the emulsifier is added;
• the optical brightener is dissolved in an organic solvent that is mostly only sparingly and Water-miscible, such as cyclohexanone or butanol, the emulsifier is added;
• the optical brightener is dissolved in a water-miscible or water-miscible solvent, the emulsifier is added, and the organic solvent is distilled off.
• the amount of brightener to be used in the present process depends on its constitution and on the strength of the desired effect; in general, it is advantageously about 0.1%, though it is often possible to achieve a distinct effect with as little as 0.01%, whereas amounts in excess of 1% are practically excluded. (The percentages are referred to the Weight of the cellulose material to be brightened.
• the solution can be added in the desired amount directly to the viscose rayon spinning mass, or else a concentrated stock solution of the optical 'brightener in the emulsifier and, if desired, in the organic solvent may be prepared.
• the viscose- which may be carried out in the usual manner, especially when the spinning mass issues from the spinnerets andenters the coagulating bath, or under certain conditions partially only during after-treatments in further baths-the brightener is precipitated again from its solution in a very finely dispersed form, but most of it remains in the solidified spinning mass, in fact the more of it the less soluble it is in water.
• Example 1 One of the spinning solutions 1 to 9 described below is stirred into 987 parts of ripened viscose ready for spinning, having a content corresponding to 75 parts of cellulose, and further containing 0.75 part of titanium dioxide. The viscose is then spun in the usual manner with a coagulating bath containing sulfuric acid to form long fibers. The resulting fibrous material displays a strong brightening eifect of satisfactory to good fastness to light and very good fastness to water and washing.
• a water-insoluble brightener not in the form of a solution but of an aqueous dispersion having an average particle sibe of 0.5a, is added to the viscose, all that is achieved as a rule is a certain yellowing and no brightening effect.
• Example 4 0.075 part of the brightener of the Formula 1 or 9/ is dissolved in 10 parts of tetrahydrofuran at room temperature. This solution is mixed with 4 parts of an adduct from 8 mols of ethylene oxide with 1 mol of para-tertiary octylphenol, thoroughly agitated, and 4 parts of oleic acid are then added. Finally, the tertahydrofuran used as additional solvent is distilled otf under atmospheric or reduced pressure. The incorporation of the solution in the viscose mass is carriel out as described in Example 1.
• Example 5 0.075 part ;of the brightener of the Formula 1 is agitated with 8 parts of a reaction product from 5 mols of ethylene oxide with 1 mol of para-nonylphenol, and the resulting solution is incorporated with the viscose mass as described in Example 1.
• Example 6 0.075 part of the brightener of the Formula 9 is thoroughly mixed by being agitated with -8 parts each of the following products:
• Example 7 0.075 part of the brightener of the Formula 1 is dissolved in parts of dioxane and mixed with 8 parts of one of the following two products:
• the solution is added to viscose as described in Example 1 and the viscose spinning mass is used for the preparation of long fibers.
• Example 8 The procedure of Example 1 is used, except that the resulting, optically brightened fibers are further subjected for 30 minutes at room temperature to a bleaching operation in a hypochlorite bath containing 2 g. of active chlorine per litre of solution. This after-treatment improves the brightening effect substantially.
• Process for the manufacture of optically brightened shaped articles from regenerated cellulose comprises adding to the unshaped viscose mass a solution containing from about 0.01% to 1% weight based on the weight of cellulose, of an organic, sparingly watersoluble optical brightening agent selected from the group consisting of dibenzoxazolyl-thiophenes, 4,4'-ditriazinylaminostilbene 2,2'-disulfonic acids, coumarins and 1,4-distyrylbenzene and a nonionic emulsifying agent selected from the group consisting of addition products of ethylene oxide with higher alcohols, para-alkylphenols and higher alkylmercaptans and of the reaction product of higher fatty acids with hydroxy alkylamines, the weightratio between the optical brightening agent and the emulsified being between 1:20 and 1:500 and submitting the viscose mass to coagulation and shaping.
• an organic, sparingly watersoluble optical brightening agent selected from the
• the brightener solution contains an organic solvent for the optical brightening agent which solvent is miscible with water in all proportions.
• Process for the manufacture of fibers from regen erated cellulose which process comprises adding to the unshaped viscose mass a solution containing from about 0.01% to 1% by weight, based on the weight of cellulose, of the optical brightener having the formula on, N N 111, no-on H3 0 H H c on,
• Process for the manufacture of fibers from regenerated cellulose comprises adding to the unshaped viscose mass of solution containing from about 0.01% to 1% by weight, based on the weight of cellulose, of the optical brightener having the formula which is dissolved in dioxane, pure oleic acid and the condensation product of one mol of p-tertiary-octylphenol with eight mols of ethylene oxide, the weightratio between the optical brightener and the condensation product being between 1:20 and 1:500, subjecting the viscose mass to coagulation to produce fibers and subsequentially to the coagulation subjecting the optically brightened fibers to a chlorine bleaching treatment.

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Citations (2)

• 1964
  • 1964-09-15 CH CH1202964A patent/CH449843A/de unknown
• 1965
  • 1965-08-07 DE DE19651570076 patent/DE1570076A1/de active Pending
  • 1965-09-08 GB GB38427/65A patent/GB1076068A/en not_active Expired
  • 1965-09-14 BE BE669614A patent/BE669614A/xx unknown
  • 1965-09-14 AT AT839665A patent/AT257823B/de active
  • 1965-09-14 NL NL6511953A patent/NL6511953A/xx unknown
  • 1965-09-14 SE SE11969/65A patent/SE320757B/xx unknown
• 1968
  • 1968-02-19 US US706667A patent/US3508942A/en not_active Expired - Lifetime

Patent Citations (2)

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