Process for the treatment of cellulose

• US 5,473,061 A
• Filed: 08/30/1994
• Issued: 12/05/1995
• Est. Priority Date: 09/04/1993
• Status: Expired due to Fees

• Current Assignee: Rhone-Poulenc Rhodia AG
• Original Assignee: Rhone-Poulenc Rhodia AG
• Inventors: Lentz, Harro, Karstens, Ties, Steinmeier, Hans, Bredereck, Karl
• Primary Examiner(s): Nutter, Nathan M.
• Application Number:
  US08/298,399
• Time in Patent Office: 462 Days
• Field of Search: 536/59, 536/62, 536/63, 536/64, 536/65, 536/66, 536/67, 536/68, 536/69, 536/70, 536/76, 536/84, 536/90, 536/92
• US Class Current: 536/59
• CPC Class Codes: C08B 1/00 Preparatory treatment of cellulose for making derivatives thereof , e.g. pre-treatment, pre-soaking, activation
• CPC Class Codes: C08B 1/02 Rendering cellulose suitable for esterification esterification per se, C08B3/00, C08B5/00, C08B7/00 or C08B9/00

Abstract

The process for the treatment of cellulose for activation for subsequent chemical reactions by bringing the cellulose in contact with liquid ammonia at a pressure higher than atmospheric pressure in a pressure vessel and subsequent expansion by rapid reduction of the pressure to atmospheric pressure, is carried out by using a cellulose pulp of an alpha-cellulose content of at least 92 mass %, letting the ammonia act on the pulp at room temperature or at a temperature higher than room temperature, after the expansion, removing the ammonia then still remaining in the pressure vessel except for a minimum content at which the state of activation reached by the action of the ammonia is still maintained and finally replacing the residual ammonia still needed to maintain the state of activation by another swelling or inclusion agent. The process is suitable, also on a large industrial scale, especially for the activation of pulp subsequently to be acetylated and makes possible to achieve a homogenous and high-grade activation. Further, no costly cooling apparatus is needed.

Claims

1. A process for treatment and activation of cellulose for subsequent chemical reactions which comprises the steps of:

a) contacting cellulose pulp of an alpha-cellulose content of at least 92 mass % with liquid ammonia at a pressure higher than atmospheric pressure in a pressure vessel at room temperature or at a temperature higher than room temperature, to obtain said cellulose pulp in the activated state;

b) allowing the ammonia to expand and escape by suddenly reducing the pressure in said pressure vessel to atmospheric pressure, removing the ammonia still remaining in the pressure vessel, except for an amount of residual ammonia necessary to maintain said cellulose pulp in the activated state which is maintained in contact with said cellulose pulp;

c) maintaining said state of activation by replacing said residual ammonia by addition of a swelling or an inclusion agent other than ammonia.

2. The process according to claim 1, wherein in step a) the ratio of the amount of liquid ammonia to said cellulose pulp is 6 mass units ammonia to 10 mass units pulp up to 10 mass units ammonia to 10 mass units pulp.

3. The process according to claim 1 wherein in step a) the temperature is 20°

C. and the pressure is 6 bars.

4. The process according to claim 1, wherein removal of said ammonia remaining in the pressure vessel in step b) is carried out by suction, pumping off or blowing off.

5. The process according to claim 1, wherein removal of said ammonia in step b) is carried out by heating the content of the pressure vessel to a temperature which at least corresponds to room temperature.

6. The process according to claim 1, wherein in step b) the amount of residual ammonia still needed to maintain the state of activation is 2 to 4 mass % ammonia with reference to the mass of pulp.

7. The process according to claim 1, wherein said swelling or inclusion agent in step c) is a member selected from the group consisting of water, steam, superheated steam, an ether, an epoxide, a glycol, a hydrocarbon, a rare gas and carbon dioxide.

8. The process according to claim 7, wherein said swelling agent is steam.

9. The process according to claim 8, wherein said steam is at a pressure of 4 bars at a temperature of 145°

C.

10. The process according to claim 1, wherein gaseous ammonia escaping during the expansion in step b) is collected and recompressed to liquid ammonia.

11. The process according to claim 7 wherein said swelling or inclusion agent is introduced into said pressure vessel, said pressure vessel has a valve, the valve is closed and then said valve is opened and said residual ammonia evaporates when said valve is opened.

12. The process according to claim 1, wherein one of the subsequent chemical reactions is acetylation of said cellulose.