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US2444022A - Process of making a solution of cellulose - Google Patents

Process of making a solution of cellulose Download PDF

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Publication number
US2444022A
US2444022A US700354A US70035446A US2444022A US 2444022 A US2444022 A US 2444022A US 700354 A US700354 A US 700354A US 70035446 A US70035446 A US 70035446A US 2444022 A US2444022 A US 2444022A
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Prior art keywords
cellulose
solution
solutions
hydrogen peroxide
sodium
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Expired - Lifetime
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US700354A
Inventor
Buurman Aart
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Akzona Inc
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American Enka Corp
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B1/00Preparatory treatment of cellulose for making derivatives thereof, e.g. pre-treatment, pre-soaking, activation
    • C08B1/003Preparation of cellulose solutions, i.e. dopes, with different possible solvents, e.g. ionic liquids

Definitions

  • Patented June 29, 1948 Fries PROCESS OF MAKING A SOLUTION OF CELLULOSE v Buurman, 'Velp, Netherlands, assignor to American Enka Co rporation, Enka, N. 0., a corporation of Delaware No Drawing. Application September 30, 1946, Serial No. 700,354. .In Germany June 27, 1941 Section 1. Public Law 690, August 8, 1946 Patent expires June 2'7, 1961 i 11 Claims.
  • the present invention relates to the manu-' iacture oi cellulosic solutions to be employed in the production of threads, filaments, films and the like, and more particularly to a method of preparing alkali metal salt solutions 04 soda celhereinafter generically referred to as cellulose.
  • the cellulose is first heated to a temperature of about 115 C. and then cut up and finally dissolvedat a temperature of about 0 C.
  • the celulose can also be chemically degraded by treatment with bisulphite solutions under pressure or by treatment with dilute sodium hydroxide followed by a substantial ripening.
  • Such degraded cellulose can then be dissolved in solutions of sodium zincate or sodium stannate by cooling the mixture to 0 C. or below, and maintaining this low temperature until complete dissolution 01' the cellulose fibers, whereupon the solutions are warmed up quickly to room temperature and formed into artificial products.
  • the present invention contemplates a process of forming cellulosic solutions of an alkaline metal salt wherein it is unnecessary to degrade the cellulose by prolonged treatment with bisulphite solutions under pressure or by treatment with the dilute sodium hydroxide solution followed by ripening,
  • inz aldehyde may be added stage in the process.
  • the time required for the degradation of the cellulose can also be regulated by utilizing a constant temperature at which the degradation takes place, or by using catalysts or by both fixing the temperature and using a catalyst.
  • the present invention represents a substantial simplification of the known methods of preparing these stypes oi solutions wherein both the old and the new methods degrade the cellulose to a measured extent prior to the formation of the soution. It is a,
  • Example 1 3350 gms. or sodium zincate solution at 25 C. containing 9.3% NaQH and 2.3% Zn. wasmixed with 330 gms. hydrogen peroxide (3%) and the mixture was thoroughly stirred. 320 gms. of cut troduce normal cellulose, i. e., soda cellulose, sulphite cellulose, or cotton linters, immediately into a dilute alkaline solution of sodium zincate or sodium stannaite containing an oxidizing agent.
  • normal cellulose i. e., soda cellulose, sulphite cellulose, or cotton linters
  • an oxidizing agent such as hydrogen peroxide is first mixed with a dilute solution of sodium zincate or sodium stannate, and uniformly cut up cellulose is introduced with stirring. The mixture forms a thick pulp which is left standing until the desired degree of degradation of the cellulose is reached. Then the known procedure is followed, namely,
  • areducing agent such as formaldehyde
  • suitable chemicals for example, areducing agent such as formaldehyde may be added so as to prevent further degradation or the cellulose.
  • areducing agent such as formaldehyde
  • the formpulp was cooled down to -,7 C. resulting in dissolution of the cellulose.
  • the solution was then warmed up to 16 C. and was in proper condition for spinning. Further degradation of the cellulose by an excess of hydrogen peroxide was prevented by adding 5cm of formaldehyde.
  • the spinning solution obtained in this manner was stable and easily spinna-ble.
  • Example 2 20 mg. of, nickel sulphate was added to 3650 to the solution either before cooling the cellulose pulp or at a later l 3 What is claimed is:
  • a process for the manufacture of cellulosic filaments, films and the like which comprises adding hydrogen peroxide to a dilute alkali metal salt solution of the class consisting of alkaline zincate and stannate solutions, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade sufllciently at a constant temperature and in the presence of nickel sulphate and then cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved.
  • a process for the manufacture of cellulosic solutions to be used in the production of threads, filaments, films and the like which comprises adding hydrogen peroxide to a dilute alkali metal salt solution of the class consisting of alkaline zincate and stannate solutions, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade sufliciently, destroying the excess hydrogen peroxide with formaldehyde to prevent further degradation of the cellulose, and
  • a process for the manufacture of cellulosic solutions to be used in the production of threads, filaments, films and the like which comprises adding hydrogen peroxide to a dilute alkali metal salt solution. of the class consisting of alkaline zincate and stannate solutions, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degradesufliciently at a constant temperature and in the presence of nickel sulphate, destroying the excess hydrogen peroxide with formaldehyde to prevent further degrade tion'of the cellulose and then cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved.
  • a dilute alkali metal salt solution of the class consisting of alkaline zincate and stannate solutions
  • a process for the manufacture of cellulosic solutions to be used in the productions 0! threads, filaments, films and the like which comprises adding hydrogen peroxide to a dilute sodium zincate solution at approximately 25 C., mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade for about 48 hours at the same temperature, cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved and then raising the solution to room temperature in readiness for spinning.
  • a process for the manufacture of cellulosic solutions to be used in the production of threads, filaments, films and the like which comprises adding nickel sulphate and hydrogen peroxide to a dilute sodium zincate solution at approximately 25 C., mixing cellulose with the solution to form a thick pulp. allowing the cellulose to degrade for about 48 hours at the same temperature, cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved and then raising the solution'to room temperature in readiness for spinning.
  • a processfor the manufacture oi cellulosic solutions to be used in the production of threads, filaments, films'and the like which comprises adding hydrogen peroxide to a dilute sodium zincate solution at approximately 25 C., mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade for about 48 hours at the same temperature, adding sufficient formaldehyde to prevent further degradation of the cellulose, cooling the mixture below 0 C. whereupon thecellulose' is immediately dissolved and then raising the solution to room temperature in readiness for spinning.
  • filaments, films and the like whichcomprises adding hydrogen peroxide to a dilute sodium 1 zincate solution, mixing cellulose with the solu-, tion toform a thick pulp, allowing the cellulose to degrade sufilcientlyv at a constant temperatureand in the presence of nickel sulphate and'th'en-j cooling the mixture below. 0 C. whereuponthe, v
  • filaments, films and the like which comprises adding hydrogen peroxide to a dilute sodium zinc- .ate solution, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade sufilciently, destroying the excess hydrogen peroxide with formaldehyde, to prevent a further degradation of the cellulose, and then cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved.
  • filaments, films and the like which comprises.' adding hydrogen peroxide to a dilute sodium' zincate solution, mixing cellulose with the soluto adilute sodium" zincate solution at approximately 2590., mixing cellulose with the solution to form a thick pulp, allowing the cellulose to demixture below- 0 Ciiwhereupon the. cellulose is immediately dissolved andthen raising the solu- 'tionroom't m erature in. readiness for spinning.

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

Description

Patented June 29, 1948 Fries PROCESS OF MAKING A SOLUTION OF CELLULOSE v Buurman, 'Velp, Netherlands, assignor to American Enka Co rporation, Enka, N. 0., a corporation of Delaware No Drawing. Application September 30, 1946, Serial No. 700,354. .In Germany June 27, 1941 Section 1. Public Law 690, August 8, 1946 Patent expires June 2'7, 1961 i 11 Claims.
The present invention relates to the manu-' iacture oi cellulosic solutions to be employed in the production of threads, filaments, films and the like, and more particularly to a method of preparing alkali metal salt solutions 04 soda celhereinafter generically referred to as cellulose.
It is known to manufacture artificial products from alkaline solutions of sodium zincate or sodium stannate, having cellulose dissolved therein.
.lulose. sulphite cellulose, or cotton linters, etc.,
There ,are several methods of preparing-these solutions, e. g., the cellulose is first heated to a temperature of about 115 C. and then cut up and finally dissolvedat a temperature of about 0 C. The celulose can also be chemically degraded by treatment with bisulphite solutions under pressure or by treatment with dilute sodium hydroxide followed by a substantial ripening. Such degraded cellulose can then be dissolved in solutions of sodium zincate or sodium stannate by cooling the mixture to 0 C. or below, and maintaining this low temperature until complete dissolution 01' the cellulose fibers, whereupon the solutions are warmed up quickly to room temperature and formed into artificial products.
The present invention contemplates a process of forming cellulosic solutions of an alkaline metal salt wherein it is unnecessary to degrade the cellulose by prolonged treatment with bisulphite solutions under pressure or by treatment with the dilute sodium hydroxide solution followed by ripening,
It is a further object of the invention to inz aldehyde may be added stage in the process. The time required for the degradation of the cellulose can also be regulated by utilizing a constant temperature at which the degradation takes place, or by using catalysts or by both fixing the temperature and using a catalyst. I
' It can be readily seen that the present invention represents a substantial simplification of the known methods of preparing these stypes oi solutions wherein both the old and the new methods degrade the cellulose to a measured extent prior to the formation of the soution. It is a,
substantial saving to eliminate the prolonged treatments of cellulose with bisulphite solutions at high temperatures and under pressure, or
treatments with dilute sodium hydroxide, which in turn necessltatesdipping, pressing and cutting up of the cellulose fibers. Incontra-distinction, the cellulose is immediately introduced into a dilute alkaline solution of sodium zincate or sodium stannate which has-previously. been mixed with an oxidizing agent. Thus, by allowing the pulp to age in this condition, an oxidizing degradation of the cellulose takes place.
Example 1 3350 gms. or sodium zincate solution at 25 C. containing 9.3% NaQH and 2.3% Zn. wasmixed with 330 gms. hydrogen peroxide (3%) and the mixture was thoroughly stirred. 320 gms. of cut troduce normal cellulose, i. e., soda cellulose, sulphite cellulose, or cotton linters, immediately into a dilute alkaline solution of sodium zincate or sodium stannaite containing an oxidizing agent.
In the preparation of the solution, an oxidizing agent such as hydrogen peroxide is first mixed with a dilute solution of sodium zincate or sodium stannate, and uniformly cut up cellulose is introduced with stirring. The mixture forms a thick pulp which is left standing until the desired degree of degradation of the cellulose is reached. Then the known procedure is followed, namely,
up sulphite cellulose with a moisture content 01' 10% was added to this solution under constant stirring. A thick rpulp formedwhich was left standing for 48 hours at 25 C., whereafter the the 'pulp is cooled down to below 0 C. with the result that the cellulose dissolves, and the solution is then quickly warmed up to about room temperature and is in readiness for spinning. into threads, films, and the like.
During the preparation of the solution, if any excess of oxidizing agent is present, suitable chemicals, for example, areducing agent such as formaldehyde may be added so as to prevent further degradation or the cellulose. The formpulp was cooled down to -,7 C. resulting in dissolution of the cellulose. The solution was then warmed up to 16 C. and was in proper condition for spinning. Further degradation of the cellulose by an excess of hydrogen peroxide was prevented by adding 5cm of formaldehyde. The spinning solution obtained in this manner was stable and easily spinna-ble.
Example 2 20 mg. of, nickel sulphate was added to 3650 to the solution either before cooling the cellulose pulp or at a later l 3 What is claimed is:
1. A process for the manufacture of cellulosic filaments, films and the like, which comprises adding hydrogen peroxide to a dilute alkali metal salt solution of the class consisting of alkaline zincate and stannate solutions, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade sufllciently at a constant temperature and in the presence of nickel sulphate and then cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved.
3. A process for the manufacture of cellulosic solutions to be used in the production of threads, filaments, films and the like, which comprises adding hydrogen peroxide to a dilute alkali metal salt solution of the class consisting of alkaline zincate and stannate solutions, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade sufliciently, destroying the excess hydrogen peroxide with formaldehyde to prevent further degradation of the cellulose, and
then cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved.
4. A process for the manufacture of cellulosic solutions to be used in the production of threads, filaments, films and the like, which comprises adding hydrogen peroxide to a dilute alkali metal salt solution. of the class consisting of alkaline zincate and stannate solutions, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degradesufliciently at a constant temperature and in the presence of nickel sulphate, destroying the excess hydrogen peroxide with formaldehyde to prevent further degrade tion'of the cellulose and then cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved. e
5. A process for the manufacture of cellulosic to degrade sufilciently at a constant temperature and in the presence of nickel sulphate. destroying the excess hydrogen peroxide with formaldehyde to prevent further degradation of .the cellulose and then cooling the mixture below 0- C. whereupon the cellulose is immediately dissolved.
8. A process for the manufacture of cellulosic solutions to be used in the productions 0! threads, filaments, films and the like. which comprises adding hydrogen peroxide to a dilute sodium zincate solution at approximately 25 C., mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade for about 48 hours at the same temperature, cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved and then raising the solution to room temperature in readiness for spinning.
9. A process for the manufacture of cellulosic solutions to be used in the production of threads, filaments, films and the like, which comprises adding nickel sulphate and hydrogen peroxide to a dilute sodium zincate solution at approximately 25 C., mixing cellulose with the solution to form a thick pulp. allowing the cellulose to degrade for about 48 hours at the same temperature, cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved and then raising the solution'to room temperature in readiness for spinning.
10. A processfor the manufacture oi cellulosic solutions to be used in the production of threads, filaments, films'and the like, which comprises adding hydrogen peroxide to a dilute sodium zincate solution at approximately 25 C., mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade for about 48 hours at the same temperature, adding suficient formaldehyde to prevent further degradation of the cellulose, cooling the mixture below 0 C. whereupon thecellulose' is immediately dissolved and then raising the solution to room temperature in readiness for spinning.
. 11. A process for the manufacture of cellulosic solutions to be used in the production of threads, filaments, films, and the like, which comprises adding 'nickel' sulphate'and hydrogen peroxide solutions to be used in the production of threads,
filaments, films and the like, whichcomprises adding hydrogen peroxide to a dilute sodium 1 zincate solution, mixing cellulose with the solu-, tion toform a thick pulp, allowing the cellulose to degrade sufilcientlyv at a constant temperatureand in the presence of nickel sulphate and'th'en-j cooling the mixture below. 0 C. whereuponthe, v
cellulose is immediately dissolved. V
6. 'A process for the manufacture of'cellulosic solutions to be used in'the production of threads,v
filaments, films and the like, which comprises adding hydrogen peroxide to a dilute sodium zinc- .ate solution, mixing cellulose with the solution to form a thick pulp, allowing the cellulose to degrade sufilciently, destroying the excess hydrogen peroxide with formaldehyde, to prevent a further degradation of the cellulose, and then cooling the mixture below 0 C. whereupon the cellulose is immediately dissolved. 3
7. A process for the manufacture'of cellulosic,
solutions to be used in the production of threads,
filaments, films and the like, which comprises.' adding hydrogen peroxide to a dilute sodium' zincate solution, mixing cellulose with the soluto adilute sodium" zincate solution at approximately 2590., mixing cellulose with the solution to form a thick pulp, allowing the cellulose to demixture below- 0 Ciiwhereupon the. cellulose is immediately dissolved andthen raising the solu- 'tionroom't m erature in. readiness for spinning.
.1. 'N SIG V The following" references are fof record in the file of this patent: I
UNITED STATES PATENTS
US700354A 1941-06-27 1946-09-30 Process of making a solution of cellulose Expired - Lifetime US2444022A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2724632A (en) * 1954-08-09 1955-11-22 Londat Aetz Fabric Co Cyanoethylated cellulose textiles modified with chromic and periodic acids and process of making same
US2887398A (en) * 1953-09-08 1959-05-19 Leslie L Balassa Composition of cellulose and an alkali biuret metal complex

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE118836C (en) *
US646799A (en) * 1899-10-26 1900-04-03 Emile Bronnert Process of producing solutions of cellulose.
US908754A (en) * 1906-10-18 1909-01-05 Emile Crumiere Process for the production of cellulose solutions.
US1279200A (en) * 1915-01-22 1918-09-17 Viscose Co Manufacture of cellulose compounds.
FR37432E (en) * 1929-09-12 1930-12-15 Switching Device Improvements
US2289085A (en) * 1937-02-18 1942-07-07 American Enka Corp Manufacture of artificial products
US2322427A (en) * 1941-08-19 1943-06-22 Edelstein Sidney Milton Cellulose product
US2368527A (en) * 1942-09-10 1945-01-30 Sidney M Edelstein Treatment of cellulosic pulp

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE118836C (en) *
US646799A (en) * 1899-10-26 1900-04-03 Emile Bronnert Process of producing solutions of cellulose.
US908754A (en) * 1906-10-18 1909-01-05 Emile Crumiere Process for the production of cellulose solutions.
US1279200A (en) * 1915-01-22 1918-09-17 Viscose Co Manufacture of cellulose compounds.
FR37432E (en) * 1929-09-12 1930-12-15 Switching Device Improvements
US2289085A (en) * 1937-02-18 1942-07-07 American Enka Corp Manufacture of artificial products
US2322427A (en) * 1941-08-19 1943-06-22 Edelstein Sidney Milton Cellulose product
US2368527A (en) * 1942-09-10 1945-01-30 Sidney M Edelstein Treatment of cellulosic pulp

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2887398A (en) * 1953-09-08 1959-05-19 Leslie L Balassa Composition of cellulose and an alkali biuret metal complex
US2724632A (en) * 1954-08-09 1955-11-22 Londat Aetz Fabric Co Cyanoethylated cellulose textiles modified with chromic and periodic acids and process of making same

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