h2 production from plastic waste

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Fluidized-bed gasification combined continuoussorption-enhanced steam reforming system tocontinuous hydrogen production from wasteplastic

Binlin Dou a,*, Kaiqiang Wang a, Bo Jiang a, Yongchen Song a,Chuan Zhang a, Haisheng Chen b,**, Yujie Xu b

a Key Laboratory of Ocean Energy Utilization and Energy Conservation of Ministry of Education, Dalian University of

Technology, 116023 Dalian, Chinab Institute of Engineering Thermophysics, Chinese Academy of Sciences, Beijing 100190, China

a r t i c l e i n f o

Article history:

Received 18 October 2015

Received in revised form

26 December 2015

Accepted 30 December 2015

Available online xxx

Keywords:

Fluidized-bed gasification (FBG)

Sorption-enhanced steam reforming

(SERP)

Hydrogen production

Waste plastic (WP)

* Corresponding author. Tel.: þ86 411847084** Corresponding author. Tel.: þ86 108254314

E-mail addresses: [email protected] (B.http://dx.doi.org/10.1016/j.ijhydene.2015.12.10360-3199/Copyright © 2016, Hydrogen Ener

Please cite this article in press as: Dou B, etsystem to continuous hydrogen productio10.1016/j.ijhydene.2015.12.197

a b s t r a c t

This paper proposes a novel system for continuous hydrogen production from waste

plastic (WP) by fluidized-bed gasification (FBG) combined sorption-enhanced steam

reforming process (SERP). The system was operated in successive processes of several

sections: (a) gasifying a WP into a raw gas comprising CO, H2, CH4, total hydrocarbons

(THC), and small amount of HCl contaminant, etc.; (b) passing the raw gas to hydrogen

production through two moving-bed reactors by continuous SERP process over Ni-based

catalyst mixed CaO sorbent for in-situ CO2 capture and HCl removal; (c) simultaneously

regenerating CaCO3 formed and catalyst with carbons deposited in other moving-bed

reactor at the regeneration condition selected; and (d) carrying the particles of catalyst

and sorbent to continuous steam reforming and their regeneration between two moving-

bed reactors by riser. Gradually expanding chamber design of FBG reactor suitable for

different particles flow to prolong the residence times of gas and solid phases makes high

carbon conversion and the maximum value is up to 83.6% at 880 �C during FBG stage. The

combination of FBG and SERP has produced a stream of high-purity hydrogen at some

certain conditions, and about 88.4 vol % of hydrogen (H2O- and N2-free basis) was obtained

at 818 �C of FBG temperature with 706e583 �C of SERP temperature. Reduced Ni-based

catalyst efficiently converted raw gas from FBG and steam to H2, and CaO sorbent in the

moving-bed reactor are capable of reducing the HCl and CO2 to low levels at all the tem-

peratures tested.

Copyright © 2016, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights

reserved.

60.8.Dou), [email protected] (H. Chen).97gy Publications, LLC. Published by Elsevier Ltd. All rights reserved.

al., Fluidized-bed gasification combined continuous sorption-enhanced steam reformingn from waste plastic, International Journal of Hydrogen Energy (2016), http://dx.doi.org/

mailto:[email protected]

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i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n en e r g y x x x ( 2 0 1 6 ) 1e82

Introduction

Depletion of fossil fuels is creating opportunities in exploring

alternative sources of energy, and at the same time, hydrogen

is a clean energy carrier for the development of potential high

efficiency power generation alternatives such as fuel cells.

The suitable waste plastic (WP) management strategy for the

manufacture of value added products is very important aspect

of sustainable development in modern society. Economical

hydrogen production from thermal-chemical conversion of

WP as a viable renewable energy source in some ready man-

ners remain a challenge [1,2]. It is very difficult for the design

and operation of conversion systems due to various compo-

sitions of WP, and the differences in its thermal degradation

behavior. Some limitations in fluidized-bed gasification (FBG)

of WP still need to be tackled to increase the feeding conver-

sion and decrease the contaminants in the gas products [3]. As

we know, the continuous removal of CO2 by CaO sorbent from

the water-gas shrift (WGS) reaction will incessantly drive the

equilibrium-limited WGS reaction in the forward direction,

which will ensure a high yield and purity of H2 with near

stiochiometric amount of steam needed for the reaction [4,5].

In addition, HCl gas contaminant from WP conversion can

simultaneously be removed by solid sorbents including CaO at

high temperatures [6].

A few papers specifically reported FBG to syngas and en-

ergy production [7e9], and the attention should be directed

towards achieving high carbon conversion and obtaining the

desire products. Seven mixtures of coals, plastics and wood

have been fed into a pre-pilot scale fluidized-bed gasifier in

order to investigate the main aspects of the co-gasification of

these materials, and the raw gas consists of CO, H2, CO2, CH4,

CnHm, etc [8]. Ruoppolo et al. reported the results of gasifica-

tion tests using a catalytic fluidized-bed gasifier to obtain a H2-

rich stream and only 32 vol% of hydrogen concentration was

produced [9]. It has been indicated that the composition of the

gas products fromgasification depends on the inherent nature

of the feeding and the process conditions employed, the

concentration of raw gas components is very difficult to adjust

and control. Tar and heavy hydrocarbons produced during

FBG of WP are undesired and dangerous for typical post-

process applications.

In the past few decades, the extensive studies on novel

systems for low-cost hydrogen production have been carried

out and the sorption-enhanced steam reforming process

(SERP) with in-situ CO2 capture has been considered to change

the normal equilibrium limits of WGS reaction for producing

high-purity hydrogen and reducing the number of processing

steps required for subsequently separating CO2 [10e13].

Recently, we reported a approach on continuous SERP [14,15]

to high-purity hydrogen production and the process was

characterized by a continuous flow concept of catalyst and

sorbent for steam reforming and regeneration using two

moving-bed reactors by the integration of continuous steam

reforming, WGS, CO2 capture, and hydrogen separation in one

single reactor, which can result in improved process efficiency

and reduced capital costs. The operating flexibility of contin-

uous SERP by two moving-bed reactors makes it possible to

utilize different types of gas and liquid feedstock such as raw

Please cite this article in press as: Dou B, et al., Fluidized-bed gasificsystem to continuous hydrogen production from waste plastic, Int10.1016/j.ijhydene.2015.12.197

gas including CO, H2, CH4, total hydrocarbons (THC), etc. from

FBG of WP. Our previous researches were directly related to

high temperature pyrolysis, and gasification [16,17], and some

reasonable amounts of gas productswere produced during the

processes.

To our knowledge, there is hardly any publication in the

literature providing information on the ways of integrating

FBG and continuous SERP for hydrogen production from a

typical WP, which is not very needed to consider the compo-

sition of the raw gas produced from FBG. The integrated sys-

tem indeed consolidates several unit operations including FBG

of WP, steam reforming of raw gas, WGS, in-situ CO2 capture

and HCl removal. Fundamental studies and experimental

works are also developed for high quality energy production

from low-cost fuels as well as the reduction of environmental

impact.

Experimental

Preparation of WP

Samples of WP from industrial plastic plant in China were

prepared in order to obtain fine particles and sieved to

0.5e1.2mm. The proximate analysis was carried out using the

method described by ASTM D5142. The ultimate analysis was

conducted using an element analyzer (EA1110, CE instru-

ment). Thermogravimetric analysis (TGA) for WP pyrolysis

was carried out using a StantoneRedcroft thermogravimetric

apparatus (STA 780). The calorific value of the sample (LHV)

was calculated by the Dulongs equation:

LHV ¼ HHV � 600 ð9HþWÞ

where; HHV ¼ 8100Cþ 34000

�H� O

8

�þ 2500S

Preparation of catalyst and sorbent

TheNiO/NiAl2O4 catalyst was prepared by the co-precipitation

method with rising pH technique under controlled conditions

and the calcination at high temperature of 900 �C in previous

studies [14]. The 1MNH4OHwas added to an aqueous solution

(Ni(NO3)2�6H2O and Al(NO3)3�9H2O) with vigorous stirring. The

precipitation was carried out at 50 �C until the final pH of 8.5

was kept. The precipitates were filtered and followed by dry-

ing at 110 �C over 15 h, and then calcined in air atmosphere at

the temperature of 900 �C for over 3 h. The spinel composition

of NieAl oxides was formed at the calcination temperature of

900 �C by the solid state reactions. The NiO content in the

catalyst is about 29.6 wt% by elemental analysis. CaO sorbent

was prepared from limestone decomposition, and it mainly

consisted of higher than 96 wt% CaO based on the data pro-

vided by the industry manufacturer. Other compounds are

CaCO3 (<2.0 wt%) andMgO (<1.0 wt%). The particles of catalyst

and sorbent in all the experiments were 0.10e0.25 mm.

Characterization of catalyst

The specific surface areas of fresh catalyst and sorbent were

determined using a Micrometric Acusorb 2100E apparatus

ation combined continuous sorption-enhanced steam reformingernational Journal of Hydrogen Energy (2016), http://dx.doi.org/



i n t e rn a t i o n a l j o u rn a l o f h y d r o g e n en e r g y x x x ( 2 0 1 6 ) 1e8 3

with BET method. For the transmission electron microscope

(TEM) analysis by a Philips Tecnai Tecnai G2 F20S-TWIN

200KV, the sample of fresh catalyst were ground and

dispersed with ethanol and deposited on a Cu grid covered

with a perforated carbon membrane. The X-ray powder

diffraction spectra were performed for fresh catalyst and

catalyst after reaction by a Shimadzu XRD-6000 powder

diffractometer, where a Cu target Ka-ray (operating at 40 kV

and 30 mA) was used as the X-ray source.

Fig. 1 e Fluidized-bed gasification combined sorption


Apparatus

Fig. 1 showed a schematic of the experimental system and

apparatus, which presented combined concept of FBG and

SERP. It primarily consisted of raw gas and H2 production, as

well as CO2 and HCl removal. FBG furnace with 30e60 mm in

ID and 800 mm in length was made of a dense alumina

ceramic tube. A diagram of FBG is also shown in Fig. 2. The

expanding chamber design of FBG reactor, which is very

-enhanced steam reforming system (FBGSERP).




Fig. 2 e The details of FBG reactor.

Table 1 e Characteristics of WP sample.

Proximate analysis wt, %

Moisture 0.51

Volatile matter 62.35

Fixed carbon 18.05

Ash 19.09

Ultimate analysis wt, %

C 65.18

H 15.61

O 9.15

N 0.16

S 0.11

Cl 2.98


suitable for different particles flow, is to prolong the resi-

dence times of gas and solid phases. Sand particles of

300e500 mm were used as FBG bed materials. The hydrody-

namics of fluidization, and chemical reactions in FBG

reactor were studied based on the EulerianeEulerian two-

fluid approach by laminar finite-rate model in the previous

studies [18,19]. The gas-solids mixture and flow, fluidized-

bed expansion and pressure drop were predicted for

different inlet gas velocities, the results indicated the gas-

solids flow system exhibited a more heterogeneous struc-

ture, and the core-annulus structure of gasesolids flow led

to back-mixing and internal circulation behavior. This has

been suggested the expanding chamber can also increase

the mixture of gases and solids. FBG process of WP particles

to raw gas was performed at a constant temperature in an

inert atmosphere of pure nitrogen (500 ml/min at STP) and

steam (500 ml/min at STP). The FBG furnace was heated to a

certain temperature and WP of 10e20 g/hr carried by ni-

trogen was injected to FBG furnace. The steam is injected at

250 �C from a steam generator. A tubular electric furnace


was used to heat and maintain FBG furnace at the required

temperature. The moving-bed reactors for continuous SERP

process has been reported in the previous studies [14,15],

and the system included two moving-bed reactors and riser.

Raw gas from the buffer bottle was injected a moving-bed

reactor. The tube in SERP reactor is about 0.012 m (ID), and

was placed in an oven with temperature control. The initial

temperature of SERP reactor was about 500 �C and SERP

reactor for a typical experiment was heated by high tem-

perature of raw gas from FBG process. The regeneration

temperature in another moving-bed reactor was kept at

900 �C. The reactant vapors in H2 production were diluted

with N2 carrier gas of 5.0 � 10�3 m3/min. The catalyst and

sorbent mixture of 50e60 g with the mass ratio of 1:1 were

introduced to SERP reactor. The moving velocity of catalyst

and sorbent particles was about 9e11 cm/min. The riser was

used for particles transport between two moving-bed re-

actors by high pressure N2. The buffer tank and some valves

were used to adjust the amount of raw gas into a moving-

bed reactor for SERP. Before the experiments, Ni-based

catalyst bed was reduced by H2 of 5.0 vol% and N2 90 vol%

for 2 h at 600 �C. The gaseous products collected in the

sample bag were analyzed off-line by a gas chromatograph

(GC) equipped with two columns connected in series (MS

and Poraplot Q) with thermal conductivity and flame ioni-

zation detectors (TCD-FID). Total gaseous hydrocarbons

(THC), which were the sum of CiHj (2 < i < 6) were also

detected by GC. The purities were calculated on dry and N2-

free basis by volume concentration ratio. The gaseous

effluent from the reactors was analyzed for HCl content by

dissolving the HCl vapor in a solution of NaOH [6].

Results and discussion

Analysis and pyrolysis of WP

The characteristics of WP samples are summarized in Table

1. First, the isothermal pyrolysis of 25 mgWP was carried out

by TGA at the temperature of 700 �C. The concentrations of

different gases only from WP pyrolysis were measured using

GC analyzer. Fig. 3 shows the degree of weight change and

pyrolysis conversion versus time. Table 2 shows the con-

centrations of gaseous compounds from WP pyrolysis. It can

be observed from Fig. 3 that the weight decreased sharply




Fig. 4 e TEM of fresh catalyst.

Fig. 3 e Weight change and pyrolysis conversion vs. time.


and theweight changemainly occurred between 1 and 6min.

The final solid residues obtained were 23% of the initial

weight. It is observed that pyrolysis gases consisted mainly

of CO, CH4 and ethylene, and the concentrations of H2 was

small, and the amount was only about 6.9%. The actual re-

action of WP pyrolysis at high temperature is extremely

complex due to the formation of many intermediate prod-

ucts. The mass loss during pyrolysis could be attributed to

the evolution of volatile matter, with further decomposition

to char and tars.

Characterization of fresh catalyst

The specific surface areas of catalyst and sorbent with the

BETmethod were 56.3 and 6.2 m2/g, respectively. TEM results

in Fig. 4 indicated the presence of small isolated particles of

NiO with a narrow particle size distribution centered at

1.6 ± 0.5 nm. It may be concluded that the dark particles were

due to the presence of NiO particles supported on the sur-

faces. XRD spectra for the fresh catalyst and catalyst after

reaction were shown in Fig. 5. The XRD results showed that

the phases in the fresh catalyst were still present in the

Table 2 e Concentrations of pyrolysis gas compounds.

Species Molecular formula Mole fraction (%)

Hydrogen H2 6.9

Carbon monoxide CO 12.6

Carbon dioxide CO2 6.7

Methane CH4 21.1

Ethylene C2H4 11.6

Ethane C2H6 6.3

Propane C3H8 5.9

1,3-Butadiene C4H6 7.5

N-Butane C4H10 5.3

1,3-Pentadiene C5H8 3.9

N-Pentane C5H12 3.1

1-Hexene C6H12 0.6

Others e 8.5

Total 100


sample after reaction, and NiAl2O4 spinel phase was detected

in two samples. NiAl2O4 in the catalyst was not reduced by H2

at the selected condition. While some peaks for Ni was

observed in the sample after reaction, these Ni peaks were

not present in the fresh catalyst with the oxidized form of

fresh catalyst, indicating that Ni has been completely

oxidized to NiO during the preparation process. Wu et al.

studied NiO/Al2O3 catalyst with the moderate Ni reduction

degree and small size of nickel particles has high activity for

catalytic steam reforming [20].

Continuous H2 production from FBGSERP system

The steady state conditions for continuous hydrogen pro-

duction from FBGSERP system were achieved within 30 min.

After that, the content of each gas component remained

rather stable. The effect of temperature on the raw gas and

hydrogen production from FBGSERP of WP was showed in

Fig. 6. The FBG experiments were carried out at the tem-

peratures of 810, 846 and 880 �C. Fig. 6(a), (c), (e) showed the

concentrations of CO, H2, CH4, HCl and THC in raw gas from

FBG at various temperatures. CO, THC and HCl in raw gas

Fig. 5 e XRD of fresh catalyst and catalyst after reaction.




Fig. 6 e Raw gas, temperature and gaseous products in FBGSERP system: (a), raw gas from FBG stage at 880 �C of FBG

temperature; (b), temperature and gaseous products from SERP stage at 880 �C of FBG temperature; (c), raw gas from FBG

stage at 846 �C of FBG temperature; (d), temperature and gaseous products from SERP stage at 846 �C of FBG temperature; (e)

raw gas from FBG stage at 818 �C of FBG temperature; (f), temperature and gaseous products from SERP stage at 818 �C of FBG

temperature.


were increased with temperature increasing. The CO

observed can also be attributed to many factors such as the

decomposition of organic compounds to produce CO and

the reverse WGS, and these reactions are favored at high

temperatures. Fig. 7 showed the values of carbon conver-

sation, CO/H2 and CO/CH4 during FBG stage. The carbon

conversion of FBG was increased with temperature

increasing and the maximum value was up to 83.6% at

880 �C. Gradually expanding chamber design of FBG makes

high carbon conversion due to prolong the residence times

of gas and solid phases. The value of CO/H2 in the range of

1.15e1.77 was increased with increasing temperature. The

CO/CH4 was about 3.71e4.27. CO2 in raw gas was not

detected from steam gasification of WP. Temperature


should be a key parameter during FBG of WP. At high tem-

perature, the steam gasification and partial decomposition

of the organic compounds from WP could produce the more

H2, CO and other gaseous products. According to

literature reported [21e24], the use of steam in gasification

process allows to foster the chemical reactions promoted by

steam, such as carbon steam gasification and hydrocarbon

steam reforming, in which the ultimate effect should be the

enrichment of gaseous products in its H2 and CO contents.

Such effect was shown clearly in Fig. 6 where a comparison

among the compositions of the product gases is presented

by taking into account the mean value of each permanent

gas component at the steady state, and calculated on dry

and N2-free basis. The slag from FBG showed the aggregate




Fig. 7 e Carbon conversion and products ratios in FBG

stage. Fig. 8 e H2 purity and HCl removal from FBGSERP system.


formation and a strip structure. During FBG process, pyrol-

ysis and gasification occurred to the volatiles and char,

resulting in the formation of soot particles, which deposited

on the wall of the reactor. A typical slag analyzed consisted

of carbon of 4e6 wt % and ash. The calculation of carbon

element balance during FBG stage showed a loss of 7e10 wt

% carbon, which may be total heavy hydrocarbons (CiHj,

i > 6) and carbon particles in raw gas.

However, a crucial requirement of the process is that raw

gas containing CO, H2, CH4, THC, heavy hydrocarbons and

carbon particles can effectively convert to H2 with in-situ

CO2 capture and HCl removal in SERP stage. In the pro-

posed system on continuous production of hydrogen from

WP by FBGSERP, the mixture of NiO/NiAl2O4 and CaO sor-

bent was moved continually by the velocity of 9e11 cm/

min between two moving-bed reactors, and the operation

for H2 production was not needed to stop for generation

both sorbent and catalyst. In a typical experiment, the SERP

reactor was preheated to initial temperatures of 500 �C. Theheating was turn off when the temperature of SERP reactor

was up to its initial temperature and the reforming reactor

was then heated by high temperature gas from FBG stage. A

mixture of raw gas, N2 and steam were fed into the SERP

reactor and the value of the molar ratio of steam to carbon

in raw gas was 3.0e4.0. Fig. 6(b), (d), and (f) depicted tem-

peratures at the central of SERP reactor and gaseous prod-

ucts distribution at the different temperatures of FBG stage.

The temperatures of SERP reactor for a certain temperature

of FBG were gradually decreased, and it is due to heating

steam and endothermic reactions of steam reforming of

CH4, THC and some compositions also including carbon

particles gasification. The temperatures at SERP reactor for

initial temperature of 500 �C showed the endothermic and

exothermic reactions can achieve hydrogen production and

energy requirement in this system, and the SERP reactor

was continuously operated without heating when the value

of S/C is not higher than 3e4, while the temperature is

decreased gradually with steam-on-time and the lowest

temperature in three cases was above 580 �C. High steam


concentration is not desirable since it lowers the energy

efficiency of the process. Fig. 6(b), (c), (d) showed the

gaseous products from SERP reactor at the different tem-

peratures. The H2 concentration was related to the tem-

peratures of moving-bed reactor, at the temperature of

above 700 �C, H2 concentration was low due to CO2 produced

was not converted by CaO sorbent to a solid carbonate at

this temperature. With a decrease in the temperature of

SERP reactor, there is a great increase of in-situ CO2 removal

by CaO sorbent, and the CO2 concentration in the product

gas decreases, which can ensure a high-purity H2 produc-

tion. The results showed that CaO sorbent in the moving-

bed reactor are also capable of reducing the HCl from FBG

of WP to very low levels at the temperatures from 538 to

788 �C, and the HCl gas of above 93% can be removed from

the inlet raw gas. It can be expected that the achievable HCl

concentrations by this process are as low as the tolerance of

a specific application such as fuel cells. Very small amounts

of CO2, CH4, CO and HCl were detected in the gaseous

products. Any THC from SERP reactor was not detected,

which showed THC was converted to H2 by catalytic steam

reforming over NiO/NiAl2O4 catalyst under these conditions.

The decay in activity of Ni-based catalyst and CaO sorbent

during the continuous steam reforming and regeneration in

60 min was not observed. The study has suggested that

small Ni particle size on the surface, high nickel dispersion

and metal-support interaction were critical to its catalytic

performance [25]. The preparation method of catalyst was

beneficial to obtain high stability at high temperature, and

also maintain 1e3 nm Ni particles on the surface. This

system has the flexibility and the component of raw gas is

not needed to adjust during FBG process and it should not be

considered the compositions of WP very much. Fig. 8

showed H2 purity and HCl removal in SERP reactor.

Hydrogen production as well as in-situ CO2 capture and HCl

removal were relatively constant throughout all the tests.

This novel process simplifies hydrogen production from WP

by decreasing the need for PSA unit requirement and con-

taminants control, and has the potential to achieve high





efficiency of system with low overall footprint by combining

different processes units.

Conclusions

First, the isothermal pyrolysis ofWPwas carried out by TGA at

the temperature of 700 �C and the weight decreased sharply to

23% in 6 min. The effect of temperature on raw syngas and H2

production from FBGSERP of WP was determined. The carbon

conversation in FBG stage was increased with temperature

increasing and the maximum value is 83.6% at 880 �C. Thevalue of CO/H2 in the range of 1.15e1.77 was increased with

increasing gasification temperature. The H2 concentration

was related to the temperature of moving-bed SWGS reactor,

at the temperature of above 700 �C, H2 concentration was very

low due to CO2 produced is not removed. High-purity H2 was

produced in low reaction temperature due to favor SERP re-

action with in-situ CO2 removal. CaO sorbent in the moving-

bed reactor was capable of reducing the HCl from raw syn-

gas to very low levels. Continuous moving, reaction and

regeneration did not lead to great decay in the activity of

catalyst and sorbent. The novel approach on FBGSERP system

for H2 production from WP with long time is feasible.

Acknowledgment

This work is supported by the Natural Science Foundation of

China (Project Nos. 91434129, 51476022, 51276032, and

51522605).

This work was also supported by International Science and

Technology Cooperation Program of China under grant

No.2014DFA60600, and the Fundamental Research Funds for

the Central Universities (DUT15JJ(G)02).

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