Simple synthesis of highly ordered mesoporous carbon
by self-assembly of phenol–formaldehyde and block
copolymers under designed aqueous basic/acidic conditions
Mingjiang Xie, Houhuan Dong, Dongdong Zhang, Xuefeng Guo
*
, Weiping Ding
*
Key Lab of Mesoscopic Chemistry, MOE, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093, PR China
ARTICLE INFO
Article history:
Received 23 October 2010
Accepted 7 February 2011
Available online 12 February 2011
ABSTRACT
In view of the low reactivity of phenol with formaldehyde under acidic condition in the syn-
thesis of ordered mesoporous carbons, a strategy to accelerate the polymerization of phe-
nol and formaldehyde by using designed aqueous basic/acidic conditions (first weakly basic
condition then highly acidic condition) is developed. The first weakly basic condition ben-
efits the formation of hydroxymethyl phenols at 313 K. The latter highly acidic condition
mainly induces the condensation reaction between the formed hydroxymethyl phenols,
as well as the self-assembly of phenol–formaldehyde and block copolymer template. After
removal of the template, the obtained carbon exhibits highly ordered hexagonal meso-
structure with a surface area of 760 m
2
g
À1
, large pore volume (0.64 cm
3
g
À1
) and uniform
pore size (3.32 nm). This developed strategy affords a simple and highly reproducible
approach for the synthesis of ordered mesoporous carbon from the less expensive phenol
under strong acidic condition, which also provides a wide and easily accessed synthesis
condition for the further functionalization, such as the in situ introducing of metal ions.
Ó 2011 Elsevier Ltd. All rights reserved.
1. Introduction
Mesoporous materials, which possess pore size range from
2–50 nm, have attracted increasing attention for its unique
characters and potential applications since the first success-
ful synthesis of M41S-type mesoporous silicates. Among
them, porous carbonaceous materials with ordered meso-
structure also have attracted wide interests in many fields
such as sorption [1], catalysis [2,3], energy storage [4–6], elec-
trochemistry [7–10], and etc. To date, ordered mesoporous car-
bonaceous materials (OMCs) with various structures have
been successfully prepared with hard [11–16] and soft-tem-
plating methods. Generally, hard templating method employs
mesoporous silica or silicates as rigid template. The carbona-
ceous sources are introduced into the pores of the template
followed by calcinations at high temperature and then the
hard template is removed by aqueous NaOH or HF dissolution
to generate mesoporous carbon replicating the silica or sili-
cates mesochannels. While in the soft-templating method,
amphiphilic surfactant molecules, such as block copolymers,
which are soft and can be decomposed during calcination, are
used as templates. The block copolymers could form a soft
micelle structure in the synthesis solution and the micelle
could interact with the oxygen-containing carbonaceous pre-
cursors mainly via hydrogen bonding or coulombic force to
form the hexagonal mesophase. After calcination at high
temperature, the mesophase is carbonized and the block
copolymers template is removed resulting in the formation
of mesopores. Apparently, for the hard templating methods,
the multi-step and costly process is hard to be employed for
the large-scale preparation of OMCs. This deficiency has stim-
ulated the search for easy-accessed, cost-saving and repro-
0008-6223/$ - see front matter Ó 2011 Elsevier Ltd. All rights reserved.
doi:10.1016/j.carbon.2011.02.014
* Corresponding authors: Fax: +86 25 83317661.
E-mail addresses: guoxf@nju.edu.cn (X. Guo), dingwp@nju.edu.cn (W. Ding).
CARBON
49 (2011) 2459– 2464
available at www.sciencedirect.com
journal homepage: www.elsevier.com/locate/carbon