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
• • 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

• nnnmrcn FINK AND raur. nssnnmm, or ranmmrz, wns-rnnvnnmmn, GERMANY,
• These acids may be partly esterified with a monovalent aliphatic alcohol, such as methyl alcohol, ethyl alcohol, propyl alcohol or with an araliphatic alcohol, such as benzyl alcohol I or with a polyvalent alcohol, such as glycol, 30
• a dibasic acid for instance, sulfuric acid
• a suitable precipitating bath is obtainable, for instance, by mixing equimolecular parts of the alcohol with the concentrated polybasic mineral acid or with-its anhydride or with the corresponding acid chloride, care being taken that the temperature of the mixture is regulated in such a manner that the best possible yield of the ester is obtained.
• the precipitating liquid shall contain at least 30% of the acid esters in question.
• Inorganic salts which are soluble in our precipitating bath may be added, for instance, sodium sulfate, sodium bisulfate, ammonium sulfate, zine sulfate, sodium bisulfite.
• Our new precipitating baths are especially useful in the manufacture of fine artificial threads of 31 deniers and even of finer fibers from an unmatured viscose prepared from unmatured alkali cellulose, for instance, according to U. S. Patent 1,428,246. Good results may even be obtained by subjecting the alkali cellulose to a previous ripening process whereas the viscose is not allowed to mature.
• an artificial silk is obtainable which has a high luster.
• the same or similar products may be already added to the viscose itself.
• the threads may be stretched in any known manner while in the precipitating bath or after they have been removed from it, that is, between the spinning bath and the collecting device, such as a bobbin or centrifuge. Th1s may be done, for example, by choosing a longer way between the bath and the collecting device or by leading the threads over rods or rolls arranged in such a manner in the bath or between the bath and the collecting device that the threads form one or more axigles on their way, or by using a suitable thread guide or by leading them into a second bath in which they may be simultaneously freed from the adhering coagulating liquid.
• the length of the thread immersed in the spinning bath may be varied Within Wide limits, for example, from 5 to 100 centimeters, said limits depending generally upon the temperature and nature of the coagulatin bath and of the nature of the viscose solution applied.
• the drawing speed of spinning may be varied up to 7 5 meters per minute, depending partly upon the temperature and nature of the bath, partly upon the length of immersion and the thickness of the thread, partly upon the viscosity of the spinning solution and finally upon the quantity of viscose solution pressed into the precipitating bath.
• the temperature of the mixture being kept for 2 hours at 4050 C.
• the acidity of the mixture has become stable as proved by titration. From the difference between the total amountof 64-66% by weight of sulture of about 41% of acid calculated as H SO it is found that the ath contains about 18% by weight of sulfuric acid monohydrate and about 52-53% of mono-methylester of sulfuric acid, the remainder being unaltered methyl alcohol and water formed by the esterification.
• a viscose solution containing 56% of cellulose and 57% of NaOH prepared from an entirely unmatured alkali cellulose, for instance, according to U. S. Patent 1,428,246 is pressed immediately after dissolving and filtering into a precipitating bath prepared as described above. Through a spinning openin of about 0.1 millimeter diameter at a drawing speed of about 30 meters per minute the viscose pump delivers such a quantity of viscose that a thread of 1 denier is formed. The temperature of thez-bath is kept at about 1520 (1., the length of immersion being about 50-100 centimeters.
• the thread After having passed the precipitating bath, the thread is guided over rods or rolls into a second bath where it is washed with water and then to a collecting device, for instance, to a bobbin, irrigated with freshwater.
• a collecting device for instance, to a bobbin, irrigated with freshwater.
• the well washed threads are freed from sulfur, bleached and finished in the usual manner known in the viscose art.
• Example 2 The same viscose solution as mentioned in Example 1 is spun under the same conditions into thesame bath but at a bath temperature of 35 C. and a length of immersion of 15 centimeters.
• Example 3 The same viscose as described uric acid and the total aciditi of the mix- .in Example 1 is spun with a length of immersion of 30 centimeters into a coagulating bath, made by mixing of 100 kilograms of ethyl alcohol of 95% strengthvwith 200 kilograms of concentrated sulfuric acid-of 96% strength and heatin until the esterification has been finished.
• e recipitating bath contains about 49% of et yl sulfuric acid and 27% of sulfuric acid; By glass rods of suitable thickness there are im arted so much angles to the filament that spinning isstill possible. All the other conditions are the same as described in Example 1.
• Example 4 The same viscose as described in Example 1, is spun under the same conditions as. in Example 3-'but with a length of immersion of 40 centimeters into a precipitatingbath,'ma-de of 200 kilograms of technical butyl alcohol and 400 kilograms of concentrated sulfuric acid. In order to diminish the high viscosity of the finished reaction mixture 100 kilograms of water are added. The bath contains about 53% of butyl sulfuric acid and 23% of sulfuric acid.
• Example 5 The same viscose as described in Example 1, is spun with a length of immersion of 15 centimeters into a precipitating bath kept at a temperature of 1520 C. which is made in the following way follows a content 52.5% of methyl sulfuric acid and 26% of sulfuric acid in the bath.
• Ewample 6 The same viscose as described in Example 1, is pressed into abath made by introducing. 7 0 kilograms of phosphoric acid anhydride into 50 kilograms of methyl alco-' hol. The mixture, after filtering from the undissolved, titrated with baryta water, contains 46.3% of monomethyl phosphoric acid 34.9% of dimethyl phosphoric acid and 3.2%,-
• the bath temperature is 15 C. .
• the drawing speed amounts to about thirty five meters per minute.
• the viscose pump delivers such a quantity of viscosethat a thread of 1 denier is formed.
• Example 7 The same viscose and acid as described in Example 5 are used. The viscose pump however is caused to deliver the double quantity of viscose so that a thread of 2 denier is formed. The diameter of the spinning openings amounts to 0.08 millimeters.
• Example 8 The same viscose and acid as described in Example 5 are used. Butthe viscose pump is caused to deliver such a quantity of viscose, that a thread of 0.5 denier is formed. The diameter of the spinning openings amounts to 0.08 millimeters.
• E azample 10 An alkali cellulose, made by immersing one part of sulfite cellulose in 15. parts of caustic soda'solution containing 18% I of its weight of NaOH at the temperature of 13 C. for two hours after having been pressed to' the triple weight of cellulose and disintegrated, is matured four days at a temperature of 18 CJ
• the matured alkali cellulose is well xanthogenized with a quantity of carbon .disulfideamounting to 40-50% of the weight of cellulose, the formed xanthogenate beingthereafter dissolved at a temperature below +10 C. to a viscose containing 78% of cellulose and 67% of NaOH.
• the finished viscose which does notshow any ammonium chloride titer'according to Hottenroth is spun immediatelyzaccording to the arrangementand with the acid described in Example 1.
• the quantity ofviscose to be delivered from the pump and the speed of drawing must'be adapted in a manner as to form a thread of 1 denier.
• Example 10 a viscose is made containing 78% of NaOH and 10% of cellulose with the same viscosity. It is spun as described in Example 10 into the same we cipitating bath, the quantity of viscose to be delivered from the pump bein 3.2 ccm per minute. A drawing speed of about 30 centimeters per minute is maintained so that, when applying a spinning nozzle of 120 spinning openings with a diameter of 0.08 millimeters,
• the threads thu'sobtainable have a dry tensile strength of3 grams and more per denier and in' the wet state 1.8 to 3 grams per denier. Dry and wet stretching amounts to 58%. They have an'excellent soft feel and luster; the luster is a little duller than that of the usualartificial silks; their capacity of beingdyed equals to that of other viscose silk prepared in the usual manner. Owing to thelr high tensile strength, they are well fit for being worked on textile machines.
• an acid ester of poly asic mine'raLacid with an aliphatic alcohol is intended to include all products which are obtainable by partly es- Emample lie-From the same alkali cellu-,
• the process for manufacturing artificial fibers from viscose which comprises pressing. a viscose solution through a spinning nozzle into a precipitating bath containing at least 30% of-an acid ester of a poly-v basic mineral acid with an aliphatic alcohol.
• the process for manufacturing artificial fibers from viscose which comprises pressing pressing a viscose solution through a spinfuric acid ning nozzle into a precipitating bath taining at least of an acid ester of furic acid with a n aliphatic alcohol.
• the process for manufacturing artificial 'fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into aprecipitating bath con taining at least 30% of an acid ester of sulwith a monovalent aliphatic consulcial fibers from viscose, which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath obtained by esterifying about molecular proportions of sulfuric acid and of methyl alcohol.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into'a precipitating bath containing at least 30% of an acid ester of a polybasic mineral acid withan aliphatic alcohol and stretching the freshly coagulated threads.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath containing at least 30% of a methyl ester of a polybasic mineral acid, and stretching thefreshly coagulated threads.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath containing 08 at least 30% of an acid ester of sulfuric acid with a monovalent aliphatic alcohol, and stretching the freshly coagulated threads.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath containing at least 30% of sulfuric acid monomethyl alcohol, and stretching the freshly coagulated threads.
• the process for manufacturing arti' ficial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath obtained by esterifying about molecular pro ortions of sulfuric acid and of metliyl alco 01, and stretching the freshly coagulated threads.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath containing at least 30% of an acid ester of a polybasic mineral acid with-an aliphatic alcohol and immediately subjecting the freshly formed threads to a washing operation.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzleinto a precipitating bath containing at least 30% of an acid ester of a polybasic ,mineral acid with a monovalent aliphatic alcohol and immediately subjecting the freshly formed threads to a washing operation.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath containing at least 30% of a methyl ester of a polybasic mineral acid and immediately subjecting the freshly formed threads to a washmg operation.
• the process ficial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath containing at least 30% of an acid ester of sulfuric acid with an aliphatic alcohol and immediately subjecting the freshly formed threads to a washing operation.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath containing at least 30% of an acid ester of sulfuric acid with a monovalent aliphatic alcohol and immediately subjecting the freshly formed threads to a washing operation.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath obtained by esterifying about molecular proportions of sulfuric acid and of a monovalent alcohol and immediately subjecting the freshly formed threads to a washing operation.
• the process for manufacturing artificial fibers from viscose which comprises pressing a viscose solution through a spinning nozzle into a precipitating bath obtained by esterifying about molecular proportions of sulfuric acid and of methyl alcohol and immediately subjecting the freshly formed threads to a washing operation and stretching the coagulated threads.
• the process for manufacturing artificial fibers from viscose which comprises pressing a completely unmatured viscose into a precipitating bath containing at least 30% of an acid ester of sulfuric acid with a-monovalent aliphatic alcohol.
• the process for manufacturing artificial fibers from viscose which comprises pressing a completely unmatured viscose into a precipitating bath containing at least 30% of sulfuric acid monomethyl ester.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• General Chemical & Material Sciences (AREA)
• Engineering & Computer Science (AREA)
• Textile Engineering (AREA)
• Artificial Filaments (AREA)
• Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Applications Claiming Priority (2)

Publications (1)

Family

ID=25817333

Family Applications (1)

Country Status (6)

Cited By (1)

Families Citing this family (1)

• 0
  • NL NL28014D patent/NL28014C/xx active
  • BE BE357602D patent/BE357602A/xx unknown
  • NL NL29414D patent/NL29414C/xx active
• 1928
  • 1928-03-15 DE DE1928I0033810 patent/DE694419C/de not_active Expired
• 1929
  • 1929-01-17 FR FR667542D patent/FR667542A/fr not_active Expired
  • 1929-03-01 GB GB6736/29A patent/GB307829A/en not_active Expired
  • 1929-03-06 US US344910A patent/US1876890A/en not_active Expired - Lifetime
  • 1929-10-31 FR FR37545D patent/FR37545E/fr not_active Expired
  • 1929-11-01 GB GB33305/29A patent/GB339740A/en not_active Expired

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