US2105609A - Method for the production of cellulose esters - Google Patents

Method for the production of cellulose esters Download PDF

Info

Publication number
US2105609A
US2105609A US5583A US558335A US2105609A US 2105609 A US2105609 A US 2105609A US 5583 A US5583 A US 5583A US 558335 A US558335 A US 558335A US 2105609 A US2105609 A US 2105609A
Authority
US
United States
Prior art keywords
cellulose
fibrous cellulose
fibrous
nitration
esterification
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
US5583A
Inventor
Mahlon G Milliken
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.)
Hercules Powder Co
Original Assignee
Hercules Powder Co
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 Hercules Powder Co filed Critical Hercules Powder Co
Priority to US5583A priority Critical patent/US2105609A/en
Application granted granted Critical
Publication of US2105609A publication Critical patent/US2105609A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • 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
    • C08B1/02Rendering cellulose suitable for esterification

Definitions

  • This invention relates to a method for the production of cellulose esters.
  • the method in accordance with this invention is adaptable for the production of various cellulose esters such as, for example, cellulose nitrate,
  • cellulose acetate benzyl cellulose, etc. and mixed cellulose esters as, for example, cellulose acetobutyrate land the like.
  • the method in accordance with this invention involves the esterification of a mixture of non-fibrous" and fibrous cellulose. More particularly, the esterification of a mixture of regenerated cellulose and fibrous cellulose is contemplated.
  • any non-fibrous cellulose may be utilized.
  • the non-fibrous cellulose may be a cellulose regenerated from a cellulose xanthate or so-called viscose solution,
  • any suitable fibrous form of cellulose may be utilized as, for example, cotton, cotton linters, wood pulp, or the like.
  • esterification of a mixture of non-fibrous and fibrous cellulose may be effected in any desired or known manner, using the usual or desired esterification reagents, apparatus and procedure, for the production of the particular ester desired, as, for example, cellulose nitrate, cellulose acetate, etc.
  • the relative proportions of fibrous and non-fibrous cellulose for esterification may be widely varied.
  • mixtures comprising non-fibrous cellulose in amount, by Weight, within about the range 25%-75% and fibrous cellulose in amount, by weight, within about the range '75%-25% will be found efficient.
  • non-fibrous cellulose as regenerated or gelatinized cellulose, will desirably be in the form of relatively thin, small pieces.
  • the regenerated or gelatinized cellulose will be prepared by cutting a film into small pieces, desirably of uniform size.
  • the fibrous cellulose will desirably be in a loose form, though sheeted fibrous cellulose in divided form, or in the form of small pieces, may be used.
  • cellulose nitrate for example, a mixture comprising 50% of regenerated cellulose, as, for example, cellophane, cut up in small, relatively thin pieces and 50% of, for example, cotton linters, is subjected for a period of about 45 min- Application February 8, 1935, Serial No. 5,583
  • the nitration may be carried out in the usual 7 apparatus used for the nitration of cotton and 10 the subsequent removal of spent nitrating mixture, washing, stabilizing, etc. of the product may follow usual procedure and with use of usual apparatus.
  • the product will comprise a uniformly nitrated product having a nitrogen content of about 12%.
  • products having desired nitrogen content may be produced by variation of the composition of the nitrating mixture, temperature, time, etc., all as is well known to the art. 20
  • esters other than nitrate the procedures, reagents and apparatus well known to the art for the production of the various cellulose esters may be followed and used.
  • the method in accordance with this invention 30 will be found highly advantageous in that a uniformly nitrated product and one productive of excellent clear solutions will be obtained and the difiiculties heretofore met with in the esterification of non-fibrous cellulose, more particularly the difiiculty of handling, especially in nitration, in the usual apparatus will be avoided.
  • the method of effecting the uniform ester- 40 ification of non-fibrous cellulose in apparatus and under conditions usually employed for the esterification of fibrous cellulose which includes admixing 25-'75% of discrete particles of nonfibrous cellulose with -25% of fibrous cellulose and then subjecting the mixture to esterification.
  • the method of effecting the uniform nitration of non-fibrous cellulose in apparatus and under conditions usually employed for the nitration of fibrous cellulose which includes admixing 25-75% of discrete particles of non-fibrous cellulose with 75-25% of fibrous cellulose and then subjecting the mixture to nitration.
  • the method of eifecting the uniform nitration of gelatinized cellulose in apparatus and under conditions usually employed for the nitration of fibrous cellulose which includes admixing 25-75% of discrete particles of gelatinizedcellulose with 75-25% of fibrous cellulose and then subjecting the mixture to nitration.
  • the method of effecting the uniform nitration of non-fibrous cellulose in apparatus and under conditions'usually employed for the nitration of fibrous cellulose which includes admixing 25-75% of discrete particles of non-fibrous cellulose with 75-25% of wood pulp and then subjecting the mixture to nitration.

Landscapes

  • 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)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Description

Patented Jan. 18, 1938 UNITED STATES PATENT orsics No Drawing.
11 Claims.
This invention relates to a method for the production of cellulose esters.
The method in accordance with this invention is adaptable for the production of various cellulose esters such as, for example, cellulose nitrate,
cellulose acetate, benzyl cellulose, etc. and mixed cellulose esters as, for example, cellulose acetobutyrate land the like.
h In essencethe method in accordance with this invention involves the esterification of a mixture of non-fibrous" and fibrous cellulose. More particularly, the esterification of a mixture of regenerated cellulose and fibrous cellulose is contemplated.
In proceeding for the practical adaptation of this invention, any non-fibrous cellulose may be utilized. Thus, for example, the non-fibrous cellulose may be a cellulose regenerated from a cellulose xanthate or so-called viscose solution,
so from cupro-ammonium solution, a gelatinized cellulose, or the like. Likewise, any suitable fibrous form of cellulose may be utilized as, for example, cotton, cotton linters, wood pulp, or the like.
The esterification of a mixture of non-fibrous and fibrous cellulose may be effected in any desired or known manner, using the usual or desired esterification reagents, apparatus and procedure, for the production of the particular ester desired, as, for example, cellulose nitrate, cellulose acetate, etc.
In practice, the relative proportions of fibrous and non-fibrous cellulose for esterification may be widely varied. By way of example, however, mixtures comprising non-fibrous cellulose in amount, by Weight, within about the range 25%-75% and fibrous cellulose in amount, by weight, within about the range '75%-25% will be found efficient.
In practice the non-fibrous cellulose, as regenerated or gelatinized cellulose, will desirably be in the form of relatively thin, small pieces. Desirably, the regenerated or gelatinized cellulose will be prepared by cutting a film into small pieces, desirably of uniform size. The fibrous cellulose will desirably be in a loose form, though sheeted fibrous cellulose in divided form, or in the form of small pieces, may be used.
As illustrative of practical adaptation of this invention for the production of, by way of ex- .ample, cellulose nitrate, for example, a mixture comprising 50% of regenerated cellulose, as, for example, cellophane, cut up in small, relatively thin pieces and 50% of, for example, cotton linters, is subjected for a period of about 45 min- Application February 8, 1935, Serial No. 5,583
utes, at a temperature of about 44 C. to a nitrating mixture made up on the following formula:
Per cent HNO3 24.05 5 I-INOSOi 4.02
H2SO4 55.68 H2O 16.25
The nitration may be carried out in the usual 7 apparatus used for the nitration of cotton and 10 the subsequent removal of spent nitrating mixture, washing, stabilizing, etc. of the product may follow usual procedure and with use of usual apparatus.
The product will comprise a uniformly nitrated product having a nitrogen content of about 12%.
As will be obvious, products having desired nitrogen content may be produced by variation of the composition of the nitrating mixture, temperature, time, etc., all as is well known to the art. 20
In proceeding for the nitration of mixtures of non-fibrous and fibrous cellulose where the fibrous cellulose comprises wood pulp, the procedure and nitrating mixture outlined above may be used or varied in accordance with practice. 25
In the production of esters other than nitrate, the procedures, reagents and apparatus well known to the art for the production of the various cellulose esters may be followed and used.
The method in accordance with this invention 30 will be found highly advantageous in that a uniformly nitrated product and one productive of excellent clear solutions will be obtained and the difiiculties heretofore met with in the esterification of non-fibrous cellulose, more particularly the difiiculty of handling, especially in nitration, in the usual apparatus will be avoided.
What I claim and desire to protect by Letters Patent is:
l. The method of effecting the uniform ester- 40 ification of non-fibrous cellulose in apparatus and under conditions usually employed for the esterification of fibrous cellulose, which includes admixing 25-'75% of discrete particles of nonfibrous cellulose with -25% of fibrous cellulose and then subjecting the mixture to esterification.
2. The method of efiecting the uniform esterification of regenerated cellulose in apparatus and under conditions usually employed for the esr terification of fibrous cellulose, which includes admixing 25-75% of discrete particles of regenerated cellulose with 75-25% of fibrous cellulose and then subjecting the mixture to esterification.
3. The method of efiecting the uniform esterification of gelatinized cellulose in apparatus and under conditions usually employed for the esterification of fibrous cellulose, which includesadmixing 25-75% of discrete particles of gelat- 4. The method of efiecting the uniform esterification of non-fibrous cellulose in apparatus and under conditions usually employed for the' esterification of fibrous cellulose, which includes admixing 25-75% of discrete particles of non-- fibrous cellulose with 75-25% of cotton fibres and then subjecting the mixture to esterification.
5. The method of effecting the uniform nitration of non-fibrous cellulose in apparatus and under conditions usually employed for the nitration of fibrous cellulose, which includes admixing 25-75% of discrete particles of non-fibrous cellulose with 75-25% of fibrous cellulose and then subjecting the mixture to nitration.
6. The method of effecting the uniform nitration of regenerated cellulose in apparatus and under conditions usually employed for the nitration of fibrous cellulose, which includes admixing 25-75% of discrete particles of regenerated cellulose with 75-25% of fibrous cellulose and then subjecting the mixture to nitration.
7. The method of eifecting the uniform nitration of gelatinized cellulose in apparatus and under conditions usually employed for the nitration of fibrous cellulose, which includes admixing 25-75% of discrete particles of gelatinizedcellulose with 75-25% of fibrous cellulose and then subjecting the mixture to nitration.
8. The method of effecting the uniform nitration of non-fibrous cellulose in apparatus and under conditions usually employed for the nitration of fibrous cellulose, which includes admixing 25-75% of discrete particles of non-fibrous cellulose with 75-25% of cotton fibres and then subjecting the mixture to nitration.
- -9.. The method of effecting the uniform nitration of non-fibrous cellulose in apparatus and under conditions'usually employed for the nitration of fibrous cellulose, which includes admixing 25-75% of discrete particles of non-fibrous cellulose with 75-25% of wood pulp and then subjecting the mixture to nitration.
10. The method of effecting the uniform ester- :ification of non-fibrous cellulose in apparatus :and under conditions usually employed for the esterification of fibrous cellulose, which includes :admixing equal parts of discrete particles of non- :fibrous cellulose and fibrous cellulose and then subjecting the mixture to esterification.
11. The method of effecting the uniform nitration of non-fibrous cellulose in apparatus and under conditions usually employed for the nitration of fibrous cellulose, which includes admixing equal parts of discrete particles of non-fibrous cellulose and fibrous cellulose and then subjecting the mixture to nitration.
' MAHLON G. MILLIKEN.
US5583A 1935-02-08 1935-02-08 Method for the production of cellulose esters Expired - Lifetime US2105609A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US5583A US2105609A (en) 1935-02-08 1935-02-08 Method for the production of cellulose esters

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US5583A US2105609A (en) 1935-02-08 1935-02-08 Method for the production of cellulose esters

Publications (1)

Publication Number Publication Date
US2105609A true US2105609A (en) 1938-01-18

Family

ID=21716609

Family Applications (1)

Application Number Title Priority Date Filing Date
US5583A Expired - Lifetime US2105609A (en) 1935-02-08 1935-02-08 Method for the production of cellulose esters

Country Status (1)

Country Link
US (1) US2105609A (en)

Similar Documents

Publication Publication Date Title
GB317608A (en) Manufacture of artificial materials from viscose
US2105609A (en) Method for the production of cellulose esters
GB369512A (en) Manufacture of viscose
US2105627A (en) Process of nitrating cellulose
US2164416A (en) Process for the production of cellulosic products
US2410319A (en) Method of producing nitrocellulose
US1415040A (en) Process for the preparation and preservation of viscose solutions of cellulose for the production of films, threads, and filaments
US1569692A (en) Preparation of alkali celluloses
DE400190C (en) Process for the production of pulp esters
US1946645A (en) Method for the production of low viscosity cellulose derivatives
US2159643A (en) Method for producing cellulose esters
DE388633C (en) Process for the production of cellulose ester solutions and masses
DE634938C (en) Process for the production of nitrocellulose
US1729628A (en) Process of conditioning cellulosic material for preparation of cellulose derivatives and product of same
US1544809A (en) Method of treating cellulose compounds
SU43153A1 (en) Method for producing purified low viscosity fiber for the production of cellulose ethers and esters
US2399620A (en) Manufacture of cellulose nitrate
US1544810A (en) Method of treating cellulose compounds
GB458467A (en) Process for the manufacture of nitro-cellulose
US1872181A (en) Method of making nitrocellulose
GB303006A (en) Manufacture of cellulose esters
US1964017A (en) Utilizing purified musa fiber cellulose
DE680685C (en) Sealing insert
DE858695C (en) Process for the production of highly viscous organic cellulose esters
US1957180A (en) Method for digesting nitrocellulose