JP2011215630A5 - Method for producing cellulose diacetate for retardation film - Google Patents

Description

That is, the present invention provides an activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is present in an acetylation solvent in the presence of an acetylation catalyst. Under the acetylation step (B) for acetylation with an acetylating agent, an acetylation reaction stopping step (C) for inactivating the acetylating agent by adding a reaction terminator to the reaction system, and after stopping the acetylation reaction The aging step (D) for adjusting the total degree of acetyl substitution and the substitution degree distribution by aging and hydrolyzing the produced cellulose acetate in acetic acid and the aging reaction stopping step (E) for stopping the aging reaction are included. A method for producing cellulose diacetate, wherein in the acetylation step (B), the reaction is performed at a temperature of at least 30 to 50 ° C. for 30 to 90 minutes. To provide a phase difference film production method of a cellulose diacetate, characterized in that.
  The present invention also includes an activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is present in the acetylation solvent in the presence of an acetylation catalyst. Under the acetylation step (B) for acetylation with an acetylating agent, an acetylation reaction stopping step (C) for inactivating the acetylating agent by adding a reaction terminator to the reaction system, and after stopping the acetylation reaction The aging step (D) for adjusting the total degree of acetyl substitution and the substitution degree distribution by aging and hydrolyzing the produced cellulose acetate in acetic acid and the aging reaction stopping step (E) for stopping the aging reaction are included. A method for producing cellulose diacetate, wherein in the ripening step (D), the amount of water used for hydrolysis is 50 mol% or more and 65 mol based on the acetic acid. To provide a phase difference film production method of a cellulose diacetate, which comprises less than.
  The present invention further includes an activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is present in an acetylation solvent in the presence of an acetylation catalyst. Under the acetylation step (B) for acetylation with an acetylating agent, an acetylation reaction stopping step (C) for inactivating the acetylating agent by adding a reaction terminator to the reaction system, and after stopping the acetylation reaction The aging step (D) for adjusting the total degree of acetyl substitution and the substitution degree distribution by aging and hydrolyzing the produced cellulose acetate in acetic acid and the aging reaction stopping step (E) for stopping the aging reaction are included. It is a manufacturing method of a cellulose diacetate, Comprising: As activated cellulose to use for the said acetylation process (B), activity in the said activation process (A) To provide a method for producing a retardation film for cellulose diacetate, characterized in that use a mixture of a plurality of activated cellulose with different process conditions.
 The present invention further provides an activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is converted into an acetylation catalyst in an acetylation solvent. In the presence, an acetylation step (B) for acetylation with an acetylating agent, an acetylation reaction termination step (C) for adding a reaction terminator to the reaction system to deactivate the acetylating agent, and terminating the acetylation reaction Thereafter, at least the aging step (D) for adjusting the acetyl total substitution degree and the substitution degree distribution by aging and hydrolyzing the produced cellulose acetate in acetic acid, and the ripening reaction stopping step (E) for stopping the ripening reaction. A method for producing cellulose diacetate comprising a plurality of cellulose diacetates having different viscosities obtained through at least the steps (A) to (E). Mixing the to provide a method of manufacturing a retardation film for cellulose diacetate according to claim.
  In addition to the steps (A) to (E), the method for producing the cellulose diacetate for each retardation film further includes a fractionation step of fractionating and purifying the cellulose diacetate obtained in the aging reaction stopping step (E) ( F) may be included.

Claims (5)

An activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is treated with an acetylating agent in an acetylation solvent in the presence of an acetylation catalyst. Acetylation step (B) for acetylation, an acetylation reaction termination step (C) for adding a reaction terminator to the reaction system to deactivate the acetylating agent, and terminating the acetylation reaction. A method for producing cellulose diacetate comprising at least an aging step (D) for adjusting the total acetyl substitution degree and substitution degree distribution by aging and hydrolysis in acetic acid, and an aging reaction stopping step (E) for stopping the aging reaction In the acetylation step (B), the reaction is performed at a temperature of at least 30 to 50 ° C. for 30 to 90 minutes. Method for producing a difference film for cellulose diacetate. An activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is treated with an acetylating agent in an acetylation solvent in the presence of an acetylation catalyst. Acetylation step (B) for acetylation, an acetylation reaction termination step (C) for adding a reaction terminator to the reaction system to deactivate the acetylating agent, and terminating the acetylation reaction. A method for producing cellulose diacetate comprising at least an aging step (D) for adjusting the total acetyl substitution degree and substitution degree distribution by aging and hydrolysis in acetic acid, and an aging reaction stopping step (E) for stopping the aging reaction In the aging step (D), the amount of water used for hydrolysis is 50 mol% or more and less than 65 mol% with respect to the acetic acid. Method for producing a retardation film for cellulose diacetate characterized. An activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is treated with an acetylating agent in an acetylation solvent in the presence of an acetylation catalyst. Acetylation step (B) for acetylation, an acetylation reaction termination step (C) for adding a reaction terminator to the reaction system to deactivate the acetylating agent, and terminating the acetylation reaction. A method for producing cellulose diacetate comprising at least an aging step (D) for adjusting the total acetyl substitution degree and substitution degree distribution by aging and hydrolysis in acetic acid, and an aging reaction stopping step (E) for stopping the aging reaction And as the activated cellulose to be subjected to the acetylation step (B), the activation treatment conditions in the activation step (A) are different. Phase difference method for producing a film for cellulose diacetate, which comprises using a mixture of several of activated cellulose. An activation step (A) in which raw cellulose is treated with an acetylation solvent to activate the cellulose, and the cellulose activated by the activation treatment is treated with an acetylating agent in an acetylation solvent in the presence of an acetylation catalyst. Acetylation step (B) for acetylation, an acetylation reaction termination step (C) for adding a reaction terminator to the reaction system to deactivate the acetylating agent, and terminating the acetylation reaction. A method for producing cellulose diacetate comprising at least an aging step (D) for adjusting the total acetyl substitution degree and substitution degree distribution by aging and hydrolysis in acetic acid, and an aging reaction stopping step (E) for stopping the aging reaction A plurality of cellulose diacetates having different viscosities obtained through at least the steps (A) to (E) are mixed. Phase difference method for producing a film for cellulose diacetate that. In addition to the steps (A) to (E), the method further comprises a fractionation step (F) for fractionating and purifying the cellulose diacetate obtained in the ripening reaction stopping step (E). The manufacturing method of the cellulose diacetate for retardation films of term.