Process for the production of carbon molecular sieves

• US 4,420,415 A
• Filed: 08/21/1981
• Issued: 12/13/1983
• Est. Priority Date: 08/27/1980
• Status: Expired due to Fees

• Current Assignee: Director-General of the Agency of Industrial Science and Technology, the Ministry of International Trade and Industry of Japan (Government of Japan)
• Original Assignee: Director-General of the Agency of Industrial Science and Technology, the Ministry of International Trade and Industry of Japan (Government of Japan)
• Inventors: Kitagawa, Hiroshi, Yuki, Nakaji
• Primary Examiner(s): Konopka, P. E.
• Application Number:
  US06/294,930
• Time in Patent Office: 844 Days
• Field of Search: 252/421, 252/444, 252/445, 252/425, 423/445, 423/449, 264/29.3, 264/29.4, 264/29.7, 55/68, 55/75
• US Class Current: 502/180
• CPC Class Codes: B01J 20/20 comprising free carbon; comprising carbon obtained by carbonising processes

Abstract

Carbon molecular sieves having excellent oxygen adsorption properties may be obtained from a vinylidene chloride copolymer. The copolymer is carbonized for the removal of its chlorine components and the resulting char is pulverized. Specific amounts of a carbonaceous sintering agent such as coal tar pitch and an organic binder such as microcrystalline cellulose are then added to the pulverized product and the mixture is shaped into pellets. By thermally treating the pellets under specific conditions in a specific manner, carbon molecular sieves having pore diameters suitable for the adsorption of oxygen may be obtained. The molecular sieves are suitable for concentrating nitrogen in air.

Claims

1. In a process for the production of carbon molecular sieves, including the steps of subjecting a vinylidene chloride copolymer to carbonization conditions for the removal of its chlorine component as hydrogen chloride, pulverizing the resulting product to a grain size of 100 mesh or finer, admixing the pulverized product with a carbonaceous sintering agent and an organic binder to obtain a mixture, pelletizing the mixture, and carbonizing the resulting pellets, the improvement comprising:

said admixing step, wherein said sintering agent includes a carbonaceous material derived from petroleum or coal and capable of forming a high-strength coke upon carbonization, is used in an amount of 10 to 14% based on the weight of said pulverized product and is a member selected from the group consisting of coal tar pitch, petroleum pitch and coking coal, and said organic binder is used in an amount of from 10 to 15% based on the weight of said pulverized product and includes a tenacious organic substance capable of being partially gasified when heated, with the remaining ungasified components being carbonized, and is selected from microcrystalline cellulose, a liquid resin, waste molasses and a sulfite pulp waste liquor, and

said step of carbonizing said pellets, wherein said pellets are heated to a temperature in the range of 750°

to 1000°

C. at a heating rate of 5°

to 7°

C./min and then maintained at that temperature for 30 to 90 min;

said molecular sieve having at least 80% of its total pore volume in pores with diameters of 4 to 4.3 A.

2. The process according to claim 1, wherein said vinylidene chloride copolymer comprises a vinylidene chloride-vinyl chloride copolymer.

3. The process according to claim 1, wherein said step of subjecting said copolymer to carbonization conditions comprises heating said copolymer at a temperature of 500°

to 700°

C. in an oxygen-free atmosphere for 1 to 5 hours.

4. The process according to claim 1, wherein said sintering agent has a grain size of 100 mesh or finer.

5. The process according to claim 1, wherein the heating of said pellets up to 300°

C. is carried out at any optional heating rate and the heating of said pellets above 300°

C. is carried out at a heating rate of 5°

to 7°

C./min.