IP Library Patent Application 10719923
Patent Application
App. No. 10/719,923

Process to reduce the pre-reduction step for catalysts for nanocarbon synthesis

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Quick Facts
Patent No.
US None
App. No.
10/719,923
Abstract

A process to eliminate or reduce the pre-reduction step for catalysts for nano-carbon synthesis by first, heating a metal oxide at 5° C./min to 350-500° C. for 70-90 minutes under 10-20% hydrogen; optionally holding the temperature for 10 to 60 minutes; then initiating carbonaceous feedstock flow.

Claims (39)

1 . A method of preparing and utilizing a catalyst for nano-fiber synthesis, comprising the following steps:

a. heating a metal oxide to an initial temperature of between 400 and 500° C. in 10-20% hydrogen at a heating rate of 1-10° C./min to affect its reduction and holding for around 10-60 minutes;

b. increasing the temperature to between 550-700° C.; and

c. passing a mixture of CO/H2 over the catalyst to produce the nano-carbon fibers.

2 . The method in claim 1 , wherein the metal oxide comprises iron oxide.

3 . The method in claim 1 , wherein the metal oxide comprises a mixture of iron and copper oxides.

4 . The method in claim 3 , wherein the mixture of iron and copper oxides contains a 99:1 to 50:50 weight ratio of Fe to Cu.

5 . The method in claim 1 , wherein the metal oxides are selected from a group consisting of oxides of iron, copper, nickel, molybdenum and combinations thereof.

6 . The method in claim 1 , wherein the heating time in step (a) is less than 60 minutes.

7 . The method in claim 1 , wherein steps a and b are performed in less than two hours time.

8 . The method in claim 1 , wherein the mixture of CO/H2 is provided at 1:4 to 4:1 by volume.

9 . The method in claim 1 , wherein the mixture of CO/H2 is provided at 1:4 by volume.

10 . The method in claim 1 , wherein the carbon production rate equals or exceeds 2.5 Carbon/g catalyst/hr.

11 . The method in claim 1 , wherein the method comprises a continuous method for producing catalyst and carbon nano-fibers by reducing the pre-reduction time ofthe catalyst.

12 . The method in claim 1 , wherein the hydrogen is balanced by an inert gas.

13 . A method of producing and utilizing a catalyst for nano-fiber synthesis, comprising the following steps:

a. heating a metal oxide catalyst to an initial temperature of between 400 and 500° C. in 10% hydrogen at a heating rate of 5° C./min to affect its reduction and holding for less than 60 minutes;

b. increasing the temperature to at least 550 oc;

c. passing a mixture of CO/H2 over the catalyst to produce nano-carbon fibers.

14 . The method in claim 13 wherein the mixture of CO/H2 is provided at 1:4 by volume.

15 . The process in claim 13 , wherein carbonaceous feedstock flow to produce nano-fibers begins within one hour from when the metal oxide catalyst is brought to its initial temperature of between 400 and 500° C.

16 . A method of producing and utilizing a catalyst for nano-fiber synthesis, comprising the following steps:

a. heating a metal oxide catalyst to an initial temperature of between 400 and 500° C. in 10-20% hydrogen at a heating rate of 5° C./min to affect its reduction and holding for around 10-60 minutes;

b. increasing the temperature to at least 550° C. but no higher than 700° C.;

c. passing a mixture of CO/H2 over the catalyst to produce nano-carbon fibers.

17 . The method in claim 16 , wherein the method comprises a continuous method of producing the catalyst for nano-fiber synthesis.

18 . A method of preparing a catalyst for nano-fiber synthesis, comprising the following steps:

a. heating a metal oxide to an initial temperature of between 400 and 500° C. in 10-20% hydrogen at a heating rate of 1-10° C./min to affect its reduction and holding for around 10-60 minutes; and

b. increasing the temperature of the catalyst to between 550-700° C. for use as a catalyst in producing nano-fiber synthesis.

19 . A method of producing a catalyst for nano-fiber synthesis, comprising the following steps:

a. heating a metal oxide catalyst to an initial temperature of between 400 and 500° C. in 10% hydrogen at a heating rate of 5° C./min to affect its reduction and holding for less than 60 minutes; and

b. increasing the temperature of the catalyst to at least 550° C. for use in producing nano-carbon fibers.

20 . A method of producing a catalyst for nano-fiber synthesis, comprising the following steps:

a. heating a metal oxide catalyst to an initial temperature of between 400 and 500° C. in 10-20% hydrogen at a heating rate of 5° C./min to affect its reduction and holding for around 10-60 minutes; and

b. increasing the temperature of the catalyst to at least 550° C. but no higher than 700° C. so that the catalyst can be used to produce nano-carbon fibers.

21 . (canceled)

22 . The method of claim 18 , wherein a mixture of CO/H2 is passed over the catalyst to produce nano-carbon fibers.

23 . The method in claim 19 , wherein a mixture of CO/H2 is passed over the catalyst to produce nano-carbon fibers.

24 . The method of claim 20 , wherein a mixture of CO/H2 is passed over the catalyst to produce nano-carbon fibers.

Assignments (4)
TERMINATION AND RELEASE OF SECURITY INTEREST IN PATENT RIGHTS Recorded Nov 19, 2010
From: HSBC BANK, USA, NATIONAL ASSOCIATION
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 025408/0645 →
RELEASE OF SECURITY INTEREST Recorded May 25, 2007
From: JPMORGAN CHASE BANK SEOUL BRANCH
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 019341/0120 →
SECURITY AGREEMENT Recorded Mar 22, 2006
From: COLUMBIAN CHEMICALS COMPANY
To: JPMORGAN CHASE BANK SEOUL BRANCH
Reel/Frame 017344/0361 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 21, 2003
From: PRADHAN, BHABENDRA K.
To: COLUMBIAN CHEMICALS COMPANY
Reel/Frame 014737/0321 →