US2218029A - Process of producing articles from cellulose acetate - Google Patents

Process of producing articles from cellulose acetate Download PDF

Info

Publication number
US2218029A
US2218029A US184968A US18496838A US2218029A US 2218029 A US2218029 A US 2218029A US 184968 A US184968 A US 184968A US 18496838 A US18496838 A US 18496838A US 2218029 A US2218029 A US 2218029A
Authority
US
United States
Prior art keywords
solution
cellulose acetate
spinning
acetic acid
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
Application number
US184968A
Other languages
English (en)
Inventor
Hubert Emil
Hofmann Rudolf
Pabst Heinrch
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.)
IG Farbenindustrie AG
Original Assignee
IG Farbenindustrie AG
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
Application filed by IG Farbenindustrie AG filed Critical IG Farbenindustrie AG
Application granted granted Critical
Publication of US2218029A publication Critical patent/US2218029A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

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
    • D01F2/24—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives
    • D01F2/28—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from cellulose derivatives from organic cellulose esters or ethers, e.g. cellulose acetate

Definitions

  • This invention relates to a process of -producing shaped articles from cellulose acetate and more especially from cellulose acetate which is soluble in chloroform. It is known to produce shaped articles for instance, fibres or threads,
  • the acetic acid content of the cellulose acetate corresponds to the theoretical value of primary cellulose acetate (cellulose trlacetate), i. e., 62.5%.
  • the solutions are more easily to be spun if a slight hydrolysis has been performed 20. which, however, should not go so far as to change the solubility of the cellulose acetate; the latter should still be soluble in chloroform and substantially insoluble in acetone.
  • the acetic acidcontent ,of the cellulose acetate 2 may vary between about 59% and the theoretical value; preferably the acetic acid content is between about 60 and 61.5%.
  • neutralizing agents are, for instance, on the one hand, aliphatic bases or the salts thereof with weak acids, like 45 propylamine, isobutylamine, diisobutylamine, triethanolamine, and on the other hand, bariumhydroxide or the salts thereof with weak acids, like, for instance, barium acetate.
  • the crude cellulose acetate solution 50 is brought to a suitable cellulose acetate content. It has been found that our process is working especially well if the cellulose acetate concentration of the spinning solution is between about 12 and 16%. Furthermore, a small content of as methylene chloride and water (from about 2 to 6%) in the spinning solution has a beneficial actionon the spinning process.
  • the cellulose acetate spinning solution is heated to a temperature which is higher than the temperature of the precipitating bath. How much the spinning solution should be heated in order to establish the most favorable conditions for spinning depends somewhat on the concentration or the viscosity res ectively of the spinning solution. Ifspinning solutions of higher concentration or higher viscosity are used, they are preferably warmed to 70 to 80 or even 90 C., whereas, if working with spinning solutions of lower concentration or viscosity it may be sufficient to heat them to about 50 to 60 C.
  • the heated spinning solution is then extruded, for instance through one of the customary spinning nozzles into an aqueous inorganic salt solution which in comparison with the spinning solution is of lower temperature.
  • aqueous inorganic salt solution may be employed for this purpose which partly have been proposed already in literature, for instance, solutions of sodium acetate or calcium chloride.
  • aqueous solutions of ammonium salts may vary within wide limits, for instance, between about 10 to 30%; their temperature may go up to about 30 to 40 C.
  • the precipitating liquid is preferably caused to act on the precipitated filaments in countercurrent, the quantity and the velocity thereof being so chosen that the acetic acid content of the precipitating liquid increases up to to 30%.
  • filaments of very good mechanical and textile properties, for instance, strength, extensibility, luster and softness.
  • the acetic acid can bemore easily recovered from the solutions which themselves are of relatively high acetic acid concentration.
  • Example 1 100 parts of cellulose which have been bleached and pretreated in the usual manner are acetylated with a mixture of 2'75 parts acetic acid anhydride, 400 parts methylene chloride and 1.3 parts sulfuric acid (specific gravity 1.84). When the reaction is complete the excess anhydride is destroyed by adding 50 parts of 50% aqueous acetic acid. The solution is then hydrolized, by heating to 50 to 60 C. for 2 to 6 hours to an acetic acid content of the cellulose acetate of 60 to 61%.
  • the excess methylene chloride is distilled off, the solution brought to a content of 14% acetyl cellulose, 2% methylene chloride, 3% water and 81% acetic acid, filtrated and deaerated.
  • the solution On its way to the spinning nozzle the solution is heated in a double-walled pipe by means of hot water (of 70 to 80 C.) and spun into a 20% aqueous chloride solution of C. which is acting in countercurrent on the precipitated cellulose acetate.
  • the rate of flow of the precipitating solution is so chosen that its acetic acid content near the spinning nozzle increases up to 17 to 20%.
  • Example 2 solution is caused to act on the filaments of cellulose acetate in such a manner that its acetic acid content near the spinning nozzle increases up to 20 to 25%.
  • Example 3 A filtrated and deaerated spinning solution prepared as described in Example 1 and having a content of 13% acetyl cellulose, 2% methylene chloride, 3% water and 82% acetic acid is heated on its way to the spinning nozzle to 55 to 65 C. and spun into a bath of 15% aqueous ammonium chloride and having a temperature of 15 C., the said bath acting in countercurrent on the precipitated filaments of cellulose acetate.
  • Example 4 A spinning solution as described in Example 3 is heated before entering the spinning nozzle to '70 to 80 C. and spun in countercurrent into a 20% aqueous common salt solution of C.
  • Example 5 A cellulose acetate spinning solution as described in Example 1 is heated to 70 to 80 C. and is thereupon spun through a spinning nozzle into a 30% aqueous ammonium acetate solution oi C.
  • the cellulose acetate solution may also be spun with a similar effect into a 20% aqueous sodium sulfate solution.
  • Process of producing shaped articles from cellulose acetate soluble in chloroform which comprises heating a crude acetic acid solution as primarily obtained by acetylating cellulose to a temperature above 50 C. and spinning it into an aqueous inorganic salt solution of a temperature below C.-
  • Process of producing shaped articles from cellulose acetate soluble in chloroform which comprises hydrolizing a crude acetic acid solution as primarily obtained by acetylating cellulose until an acetic acid content of not less than 59% is reached, heating said solution to a temperature above 50 C., and spinning it into an aqueous inorganic salt solution of a temperature below 40 C.
  • Process of producing shaped articles from cellulose acetate having an acetic acid content of from 59 to 62.5% which comprises rendering the acetylation catalyst of the crude solution as primarily obtained by acetylating cellulose ineffective, bringing the solution to an acetate content of about 12-16%, heating it to a temperature above 50 C., and spinning it into an aqueous inorganic salt solution of a temperature below 40 C.
  • Process of producing shaped articles from cellulose acetate soluble in chloroform which comprises rendering ineffective the acetylation catalyst in the crude solution of cellulose acetate as primarily obtained by :acetylating cellulose, bringing the solution to an acetate content of about 12-16%, heating it to a temperature above 50 C-., said solution containing of from 2-6% of Water and methylene chloride, and spinning it into an aqueous inorganic salt solution of a temperature below about 40 C.
  • Process of producing shaped articles from cellulose acetate having an acetic acid content of from 59-62.5% which comprises rendering ineffective the acetylation catalyst contained in the crude acetic acid solution as primarily obtained by acetylating cellulose, bringing the solution to an acetate content of about 12-16%, heating it to a temperature above 50 0., said solution containing of from 2-6% of water and methylene chloride, spinning it into an aqueous inorganic salt solution of a temperature below about 40 C., and leading the said inorganic salt solution in a coun'tercurrent to the flow of the precipitated cellulose acetate.
  • Process of producingshaped articles from cellulose acetate having an acetic acid content of from 5962.5% which comprises rendering inefiective the acetylation catalyst contained in the crude acetic acid solution as primarily obtained by acetylating cellulose, bringing the solution to an acetate content of about 12-16%, heating it to a temperature above 50 C., said solution containing of from 2-6% of water and methylene chloride, and spinning it into an aqueous. solution of an ammonium salt of a temperature below about 40 C., and leading the said ammonium salt solution in countercurrent to the flow of the precipitated cellulose acetate.
  • Process of producing shaped articles from cellulose acetate having an acetic acid content of from 59-62.5% which comprises rendering inefiective the acetylation catalyst contained inthe crude acetic acid solution as primarily obtained by acetylating cellulose, bringing the. solution to an acetate content of about l2l6%, heating it to a temperature above 50 C., said solution containing of from 2-6% of water and methylene chloride, and spinning it into an aqueous solution of an ammonium salt of a temperature below about 40 C., and leading the said ammonium salt solution in countercurrent to the flow of the precipitated cellulose acetate in such a manner that the acetic acid content thereof increases up to from 15-30%.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Artificial Filaments (AREA)
US184968A 1937-01-19 1938-01-14 Process of producing articles from cellulose acetate Expired - Lifetime US2218029A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE509702X 1937-01-19

Publications (1)

Publication Number Publication Date
US2218029A true US2218029A (en) 1940-10-15

Family

ID=6547275

Family Applications (1)

Application Number Title Priority Date Filing Date
US184968A Expired - Lifetime US2218029A (en) 1937-01-19 1938-01-14 Process of producing articles from cellulose acetate

Country Status (3)

Country Link
US (1) US2218029A (enrdf_load_stackoverflow)
GB (1) GB509702A (enrdf_load_stackoverflow)
NL (1) NL46526C (enrdf_load_stackoverflow)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2687944A (en) * 1949-02-23 1954-08-31 British Celanese Manufacture of water-soluble textile and other materials
US2824035A (en) * 1954-01-12 1958-02-18 British Celanese Process of making stiffened composite fabrics

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB652844A (en) * 1948-11-24 1951-05-02 Courtaulds Ltd Improvements in and relating to the production of artificial threads, fibres, filaments, staple fibres and the like

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2687944A (en) * 1949-02-23 1954-08-31 British Celanese Manufacture of water-soluble textile and other materials
US2824035A (en) * 1954-01-12 1958-02-18 British Celanese Process of making stiffened composite fabrics

Also Published As

Publication number Publication date
NL46526C (enrdf_load_stackoverflow)
GB509702A (en) 1939-07-19

Similar Documents

Publication Publication Date Title
US4415734A (en) Process for preparation of cellulose acetate
US2126190A (en) Cellulose esters
US2218029A (en) Process of producing articles from cellulose acetate
US2214943A (en) Purification of cellulose esters
US2327516A (en) Manufacture of artificial filaments and fibers from viscose
US2265916A (en) Manufacture of shaped structures and other useful articles from cellulose derivatives
US2028761A (en) Method of treating cellulose esters of organic acids
US3755297A (en) Continuous secondary cellulose ester process
US2265918A (en) Mixed cellulose ether and process of making same
US2297613A (en) Process of producing viscose rayon
US2375650A (en) Manufacture and production of artificial filaments, threads, films, and the like
US2341586A (en) Wet spinning of cellulose acetate
US2073853A (en) Cellulose esters and production of
US2447756A (en) Process for treating cellulose ethers to improve their dissolving properties
US1379351A (en) Process of making cellulose xanthogenate solutions and product produced
US1755657A (en) Caustic-soda solution of cellulose
US1858993A (en) Process for producing cellulose esters
US2414869A (en) Process for the production of cellulose esters
DE737505C (de) Verfahren zur Herstellung einer hochkonzentrierten Loesung eines stabilen, hochviscosen, teilweise verseiften Celluloseacetates
US1866971A (en) Process of making cellulose acetate
US3498812A (en) Process for making cellulose triester spinning dope
US1742611A (en) Cellulose esters and the manufacture thereof
DE514892C (de) Verfahren zur Herstellung von Cellulosederivaten
US2592305A (en) Method of lowering the viscosity of hydrolyzed cellulose esters and product
US1857190A (en) Process for the hydrolysis of cellulose acetate