Table of Content

28 June 2019, Volume 19 Issue S1

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Cover and Contents

Chin. J. Process Eng.. 2019, 19(S1):  0. 

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Congratulations on Professor Yi Zhang's 80th birthday

Suojiang ZHANG

The Chinese Journal of Process Engineering. 2019, 19(S1):  1-2.  DOI: 10.12034/j.issn.1009-606X.219002

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今年6月11日，是张懿院士八十大寿，值此之际，中国科学院过程工程研究所经由《过程工程学报》为张懿院士发行《绿色制造的全过程污染控制》专刊，本专刊特邀多名资源、环境领域知名专家精心撰写论文，以贺张懿院士八十华诞。

Origin of process engineering and study on the irreversible circular processes

Zuohu LI

Chin. J. Process Eng.. 2019, 19(S1):  3-9.  DOI: 10.12034/j.issn.1009-606X.219214

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In the year 1996, we found that, if the closed recycling reaction between acid?alkali?salt should be completed, we can be able to zero discharge in the clean production of chemical technology process. At the beginning of the year we study the acid?alkali united production from metallic salts by hydrolytic action as a new unit operation of chemical engineering. In the year 2012, we get up the theory of dynamic closed system with multy-phase and chemical kinetics, and find the third group from entropy to order structure in the nonequilibrium thermodynamics. If the new theory expanded to the solar system, we discover the closed circular flow of entropy and universal eternal self-motive machine, so we give the new definition of the times.

Technical progress of green high-value utilization of strategic rare metal resources

Tao QI Weijing WANG Guangye WEI Zhaowu ZHU Jingkui QU Lina WANG Hui ZHANG

The Chinese Journal of Process Engineering. 2019, 19(S1):  10-24.  DOI: 10.12034/j.issn.1009-606X.219142

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Focus on resource shortage, environmental pollution, and low grade products, the major national demands of China's rare metal resources such as vanadium, titanium, nickel, cobalt, and lithium, in the era of rapid development of strategic emerging industries were summarized, and the major progress and achievements of this field in recent years through upgrading and reforming the utilization technology of vanadium-bearing titanomagnetite, laterite nickel ore, and high magnesium content brine were reviewed. The main conclusion was that: (1) Unconventional medium strengthening methods such as coal-based sodium salt smelting, high temperature carbonization?low temperature chlorination, and oxidation of sub-molten salt were the core of achieving green high-value utilization of vanadium and titanium in vanadium-titanium magnetite. (2) The hydrochloric acid leaching?low temperature selective hydrolysis?coprecipitation process was an advanced representative technology which can shortly achieve the high-efficiency and high-value utilization of all components of the laterite nickel ore with low cost. (3) Double-functional synergistic system was the key to realize the green utilization of lithium extraction and stripping from high magnesium content brine. Based on the two ideas of solid waste recycling and waste reduction at source, the utilization technology of strategic metal resources at the present stage had preliminarily solved the problems of environmental pollution and low utilization rate of resources, but there were still common problems such as the lack of basic principles of green utilization of resources and low scientific technological content of products. At the end of this work, the frontier research direction of green high-value utilization of rare metal resources guided by strategic industrial key materials was prospected, e.g. basic research on the application and value-increment of rare metal.

Development trend and prospect of green separation technology

Huizhou LIU Xiaoping LIU Xin CHEN Chao ZHANG Liangrong YANG

The Chinese Journal of Process Engineering. 2019, 19(S1):  25-34.  DOI: 10.12034/j.issn.1009-606X.219145

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Since the beginning of the 21st century, green separation technology has been continuously innovated, new green separation technologies have emerged, and application fields have gradually expanded. This paper uses bibliometric method to research the development trends of seven green separation technologies, and it analyzes the aspects of the paper's output scale, quality of research, disciplinary layout and international cooperation. Besides, the paper compares and analyzes various green separation technologies. The paper aims to compare the strength of China with the developed countries, and provides useful reference for the development of green separation technology, development strategy and discipline policy, scientific research workers to choose scientific research direction, and enterprise investment decision-making.

Control and resource recovery of industrial volatile organic compounds

Zeli WANG Xingang LI Chenggong ZHENG Lin HE

Chin. J. Process Eng.. 2019, 19(S1):  35-44.  DOI: 10.12034/j.issn.1009-606X.219159

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Volatile organic compounds (VOCs) are primary sources of atmospheric pollution. Their huge emissions cause enormous harm to both the human health and the ecological environment. Various recovery and destruction control technologies of industrial VOCs gas, including adsorption, desorption, condensation, membrane separation, regenerative thermo oxidizer (RTO), regenerative catalytic oxidizer (RCO), biofiltration, photocatalytic oxidation and non-thermal plasma oxidation, have been reviewed. Their advantages and disadvantages, range and status of industrial applications, and future research directions were analyzed from the perspective of chemical engineering. Scientific research and industrial application of various abatement methods have got lots of impressive progresses, which have greatly improved the emission reduction of VOCs. However, there are still existing some problems in the current industrial VOCs control process, such as the dilemma between recovery methods and destruction methods, the treatment of VOCs gas with low concentration, large flow rate and small VOCs molecule, the disposal of VOCs gas mixed with organic and inorganic impurity, the low efficiency of single method to control the VOCs gas and so on. The solution should be promoted by the cooperation of engineers in environmental protection field and relative chemical technology. From the technical view, the process, technology and equipment of various control methods, especially recovery methods, should be further improved. Integration and coupling of different treatment modes could improve the treatment efficiency of VOCs gas and the economic benefits while reducing the energy consumption. The best way to reduce or block the emission of VOCs was to control at the source by optimizing the equipment or find the alternatives of VOCs. It could reduce the workload in later VOCs treatment. And the reduction in unorganized emission has great significance for human health and ecological environment.

Effect of weak oxidizer CO₂(g) on the vanadium slag production from the vanadium-bearing molten iron

Zhitong SUI Taiping LOU Shouxing HUO

Chin. J. Process Eng.. 2019, 19(S1):  45-50.  DOI: 10.12034/j.issn.1009-606X.219149

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75%?85% of vanadium products in the world are produced from the vanadium?titanium magnetite, in vanadium-titanium magnetite, Fe, V and Ti are distributed in the isomorphism phase, which cannot be enriched and separated by physical methods. Usually, the vanadium slag and the semi-steel are obtained by the oxygen blowing process in the steel making process. The semi-steel is used to produce steel, and the vanadium slag is the raw material for extracting vanadium. When vanadium slag is obtained by blowing vanadium-bearing molten iron with oxygen, the impurities such as Ca, Mg, Al, Ti and Si in the molten iron enter into slag phase along with V, oxygen as a strong oxidizer. Both vanadium oxide and impurity oxides are contained in the vanadium slag, resulting in high impurity content and low vanadium grade, which make the subsequent vanadium extraction process costly, that is the drawback of the current vanadium slag process. Weak oxidizer CO2(g) was used in this research to produce the low-silicon and high-vanadium slag by selective oxidation, during which Si was removed into slag firstly and then V left in the molten iron by weak oxidation. Theoretical analysis was firstly performed and then the effects of temperature, flow rate of CO2(g), stirring and smelt agent on the desilication process were investigated. The results showed that the desilication rate reached 68.62%, and the oxidation rate of vanadium was only 0.73% when the desilication process was performed with stirring and CO2(g) flow rate of 1 L/min at 1450℃.

Nitric acid pressure leaching of laterite ores

Chengyan WANG Zhihe CAO Baozhong MA Yongqiang CHEN

Chin. J. Process Eng.. 2019, 19(S1):  51-57.  DOI: 10.12034/j.issn.1009-606X.219136

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The treatment of laterite ore by pressure leaching using nitric acid medium was studied. The nitric acid pressure leaching of nickel laterite was feasible based on series experiments for valuable components of initial concentration of nitric acid, leaching temperature, leaching duration, and liquid to solid ratio of the process. More than 85% Ni and Co, 80% Mg, over 60% Al and less than 1% Fe were extracted, and iron slag including 55% Fe was produced followed by optimal conditions of leaching temperature of 190℃, leaching duration of 60 min, initial concentration of nitric acid of 330 kg/t and liquid to solid ratio ranged from 1.5:1 to 1.7:1 mL/ g. Then Fe, Al and Ni, Co in the leaching solution were separated and enriched further, by the step of replenishing MgO. When the temperature was 85℃ and the pH was around 3.0, 95% Fe was removed. Then with controlled pH among 4.0~4.3, more than 99% Al was removed and more than 90% Sc was in the slag with Al which contained nearly 1000 g/t Sc. With increased pH among 7.5~8.0, Ni and Co were precipitated completely to produce hydroxide Ni, Co slag including 24.8% Ni and 2.3% Co. The residual Mg(NO3)2 solution was first evaporated and then thermal decomposed at 500℃ to obtain MgO. The nitrogen oxide gas generated by thermal decomposition was recovered to regenerate HNO3. The efficiency of recycled HNO3 was more than 92% in the atmospheric pressure.

Research progress on alkaline media reactive oxygen species tuning technique in hydrometallurgy

Shili ZHENG Yudong XUE Hao DU Yi ZHANG

Chin. J. Process Eng.. 2019, 19(S1):  58-64.  DOI: 10.12034/j.issn.1009-606X.219144

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The green upgrade of the chemical metallurgy manufacturing industry needs to start from the innovation of cleaner production technology. Research and development of efficient, green and reasonable utilization of major characteristic resources are the keys to realizing the sustainable development of resources and environment. Cleaner production is the best pattern of pollution preventing and the only way to achieve sustainable development and recycling economy. The sub-molten salt media clean chemical metallurgical generic technology created by Professor Yi Zhang, academician of Chinese Academy of Engineering (CAE), has realized the efficient clean conversion and separation of refractory amphoteric metal minerals with chemical commonality (including Al, Cr, V, Ti, Mn, Nb, Ta, etc.). Reactive oxygen species have been considered as the key factor to realize the efficient conversion of amphoteric metal mineral resources. The sub-molten salt media chemical system with the reactive oxygen species tuning as the core technology was established. The reactive oxygen species tuning strategy in the sub-molten salt media is summarized into five methods, including chemical field enhancement, flow field enhancement, pressure field enhancement, additive enhancement, and microbubble enhancement. All the above methods can be applied to strengthen the decomposition of amphoteric metal mineral resources and decrease the reaction conditions. Till now, the sub-molten salt technology has been successfully applied to the treatment of vanadium titano-magnetite, chromite, diasporic bauxite, tantalum-niobium ores, and high-alumina fly ash. Furthermore, as a feasible, efficient, easy operation and environment-friendly method, electrochemistry plays a vital role in various fields including metallurgy, chemical engineering, and catalysis. Based on the basic research of reactive oxygen species by electrochemical method in our group, novel alkaline electrochemical advanced oxidation processes with electrochemical reactive oxygen species tuning technology were proposed, which provides theoretical and technical support for the application of the reactive oxygen species tuning technology in metallurgy, resources and environment fields.

Alloys preparation from refractory metal oxysalts by molten salt electro-deoxidation using liquid cathode

Zhi WANG Mingyong WANG Wei WENG

Chin. J. Process Eng.. 2019, 19(S1):  65-71.  DOI: 10.12034/j.issn.1009-606X.219170

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Long processes, high energy consumption and severe pollution are the issues for the conventional metallurgy of refractory metals. Instead of the thermal reduction method, molten salt electro-deoxidation is the most promising technique to produce refractory metals. Herein, a new process is proposed for direct transforming typical refractory metal (V/Cr/Ti) oxysalts in melting state to metal or alloys by molten salt electrolysis with liquid cathode. Refractory metal oxysalts with low melting point are used as both electrolytic reactants and conductive molten salts. This innovation work would provide theoretical foundation for building universal and green method to produce refractory metals with high efficiency.

Recovery of TiO₂ from spent SCR denitration catalyst by alkali hydrothermal method

Wenfen WU Huiquan LI Ziheng MENG Chenye WANG Xingrui WANG Chen ZHAO

Chin. J. Process Eng.. 2019, 19(S1):  72-80.  DOI: 10.12034/j.issn.1009-606X.219154

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Recovery of TiO2 from spent selective catalytic reduction (SCR) denitration catalyst used in coal-fired power plants was studied by alkali hydrothermal method. The content of TiO2 as a carrier was 90%, which was the main component in spent SCR denitration catalyst. Due to the high content and suitable reaction Gibbs free energy change (ΔrG) value of WO3 in all oxide of spent SCR denitration catalyst except TiO2, it was selected as an example of impurity to remove. The effects of NaOH concentration, reaction temperature, solid to liquid ratio and stirring speed on the leaching of W element with low Ti leaching in the alkali hydrothermal process were determined by orthogonal experiment. Effect of each factor on the leaching rate of W and Ti and the change of crystal phase of the residua were further investigated. Finally, the optimal leaching conditions of separation W and recovery Ti were obtained. The results showed that the most significantly influence factors was the reaction temperature. Under the optimal leaching conditions of reaction temperature 110℃, NaOH concentration 40wt%, the ratio of solid to liquid 1/5 g/mL, stirring speed 400 r/min, the leaching rate of W reached 87.5% and Ti was 0.04%. Meanwhile, the leaching concentration ratio W/Ti was 210. Under the optimal process conditions, the crystal phase of leached residua completely changed from anatase TiO2 to amorphous titanate. The residua obtained under the optimal process conditions were washed by H2SO4 or HCl respectively in order to recover TiO2. The results showed that anatase TiO2 was generated by H2SO4 system, and rutile TiO2 was generated by HCl system. The purities of both TiO2 materials were higher than 98%. Recovery of TiO2 by alkali hydrothermal method showed a relatively low temperature (80?120℃) when the NaOH concentration was 20wt%?40wt%. It could realize the controllable recovery and utilization of titanium resources.

Co-extraction and synergistic detoxification technology and its application in high-concentration wastewater from coal chemical industry

Hongbin CAO Gaojie XU Pengge NING Shaoyuan SHI

Chin. J. Process Eng.. 2019, 19(S1):  81-92.  DOI: 10.12034/j.issn.1009-606X.219163

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High-concentration wastewater from coal chemical industry has attracted widespread attention because of complex composition, high concentration of pollutants, high toxicity and low biodegradability. It not only contains ammonia nitrogen, phenols and oil compounds with high concentration, but also contains highly toxic pollutants such as heterocyclic compounds and polycyclic aromatic hydrocarbons (PAHs). High-efficiency dephenolization and deep detoxification are the two major bottlenecks in wastewater treatment. In this work, the phenolic?oil co-extraction synergistic detoxification technology was proposed from the perspective of process pollution control, and the special extractant IPE-PO was used to treat the high-concentration wastewater from coal chemical industry in Yunnan. The organic matter in the wastewater before and after treatment was detected by GC?MS, and compared with methyl isobutyl ketone (MIBK) extraction system which was used in industrially widely. After treatment using IPE-PO extractant, the average removal rates of chemical oxygen demand (COD), total phenol, ammonia nitrogen (NH4+?N) and absorbance of organic matters at 254 ?nm (UV254) were 77.69%, 90.45%, 97.10% and 82.19%, respectively. Most of the toxic pollutants were removed, and the biodegradability of the wastewater was improved significantly. There were 101 kinds of organic matters in the raw water, after IPE-PO process, the types of organic compounds were reduced to 74 kinds. The process showed ascendancy in the treatment of toxic matters. After biochemical and advanced treatment, the COD of wastewater reduced from 31000~37000 mg/L to less than 100 mg/L, and the UV254 of wastewater reduced from 197 cm?1 to 0.5 cm?1, which meet the wastewater discharge standard of China. Compared with the MIBK extraction system, the deep detoxification ability of the technology was proved. The operating cost does not exceed 10 yuan/t wastewater. The phenol?oil synergistic co-extraction detoxification technology with IPE-PO extractant is a feasible and efficient pretreatment method for coal chemical wastewater treatment.

Vanadium extraction from vanadium removal tailings of crude titanium tetrachloride organic refining

Zhaohui SUN Ming LI Guanjin GAO Liang LI

Chin. J. Process Eng.. 2019, 19(S1):  93-98.  DOI: 10.12034/j.issn.1009-606X.219195

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In the process of preparing titanium tetrachloride by chlorination technology, vanadium oxychloride and titanium tetrachloride will be extracted and condensed at the same time. Because of the close boiling point, aluminum powder or organic substance is used to remove vanadium oxychloride from titanium tetrachloride in order to prepare titanium products such as sponge titanium, titanium dioxide and so on. The tailing produced by organic refining was a kind of high-quality raw material for vanadium extraction due to the high content of V2O5 (20wt%), and the impurity element is relatively few. In view of the extraction of vanadium from the tailing obtained by organic refining of titanium tetrachloride and the preparation of vanadium pentoxide product, the roasting temperature, the amount of leaching agent, the ratio of liquid to solid and the leaching temperature were studied. Furthermore, the effect of leaching time on the conversion rate and dissolution rate of vanadium in the tailing were studied respectively. The results showed that when calcination temperature was higher than 600℃, carbon and chlorine could be removed efficiently (<0.1%). Vanadium mainly existed in the form of vanadium pentoxide in the slag after roasting. The roasted slag was leached with sodium carbonate aqueous solution, the ratio of liquid to solid was 6 mL/g, the leaching rate of vanadium was 85.5% at 80℃ for 60 min. The leaching solution contained only a small amount of Si, Al, Ti, P impurities, which was suitable to precipitate vanadium product directly. Ammonium metavanadate was prepared by addition of ammonium salt with NH4+:V=2.5:1 (molar ratio), and stirring at room temperature for 120 min, after filtering, washing, drying and calcining to obtain vanadium pentoxide. The chemical composition of vanadium pentoxide can fully meet the requirement of grade 99 powder vanadium. The vanadium yield of the whole process was 75%.

Clean utilization of solid waste of vanadium chemical and metallurgy

Lanjie LI Beibei ZHAO Minglei GAO Litang GENG Ruiguo BAI Chaoyang LIU Xindong WANG

Chin. J. Process Eng.. 2019, 19(S1):  99-108.  DOI: 10.12034/j.issn.1009-606X.219208

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In view of the fact that the solid waste resources such as vanadium tailings, chromium mud, vanadium mud, iron vanadate mud and slag of FeV50 produced in the vanadium chemical and metallurgical industry were difficult to be utilized on a large scale, a low-cost and high-efficiency vanadium chemical smelting industry with industrialized value was developed by adopting the strategy of integrated value-added utilization, multi-component high-efficient extraction and end harmless disposal, and through the innovation and integration of key core technologies, a low-cost and high-efficiency integrated technology for clean utilization of solid waste of vanadium chemical metallurgy with industrial value has been developed. After vanadium tailings were extracted by sub-molten salt technology, V2O5 content in the final slag was reduced to below 0.2wt%, and Fe2O3 content in the final slag was enriched to over 60wt%. The Na2O content in the final slag was less than 2wt% after calcification and desalination, which could replace the low-vanadium and high-grade iron concentrate in a large proportion for ore blending and sintering, from the original 20 kg/t to 60 kg/t. The bulk and powder chromium mud was made into spherical skeleton by adding organic binder and 65 silicon carbide, processed into spherical material of 5?30 mm diameter and baked, and then added into steel-making process. Compared with conventional process, the yield strength and tensile strength were improved, which had a certain effect on improving the performance of reinforcing bars. It was feasible to use iron vanadate to partly replace vanadium pentoxide in ferrovanadium smelting. 1 t iron vanadate can replace 209 kg of vanadium pentoxide. The consumption of iron vanadium per ton was 0.2 t. The recovery rate of vanadium was over 90%. Slag of FeV50 as a "bonding" ingredient to improve the strength of V?Ti sinter, while recovering and utilizing V, Mg and Ca elements in the slag, the drum index of V?Ti sinter increased by 2%-4%.

Degradation of corn stover components with microwave torrefaction

Xia XU Yun WU Yong ZHAO Hongqiang LI Min PENG Jian XU

Chin. J. Process Eng.. 2019, 19(S1):  109-114.  DOI: 10.12034/j.issn.1009-606X.219160

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As an indispensable step in biomass utilization chain, the current pretreatment methods cannot meet the industrial production requirements of low cost, low pollution and high efficiency. New technology development is necessary. In this work, microwave irradiation-based torrefaction pretreatment was employed to investigate the degradation of the major components in corn stover with or without catalysts. In addition, the destruction and change of corn stover structure before/after pretreatment and enzymatic hydrolysis were also studied. The results showed that the monomers of the three major components (cellulose, hemicellulose and lignin) were transformed dramatically with microwave treatment. However, they were not degraded from the polymer structure. With the presence of catalysts, the microwave torrefaction presented selective degradation effect on corn stover. The addition of acid, alkali or glycerol in the pretreatment process increased the content of cellulose. NaOH was observed to be the most effective catalyst. The cellulose content increased from 33% to 42%. The contents of other components in the solids were significantly reduced. Enzymatic hydrolysis experiments on the corn stover obtained from different pretreatments. After microwave torrefaction for 20 min, the yield of glucose increased from 12% to 17% with the enzymatic hydrolysis rate of cellulose increased from 33% to 65%. NaOH as a catalyst in the pretreatment process could significantly improve the enzymatic hydrolysis rate of cellulose. The glucose yield was increased from 12% to 30%. While the enzymatic hydrolysis of the corn stover pretreated with sulfuric acid or glycerol presented a slight effect or no effect. Microwave torrefaction increased temperature without the use of pressure vessels and organic solvents compared to single microwave irradiation process. Due to the unique advantage such as easy operation and less energy consumption, the microwave torrefaction can be developed into a practical and efficient biomass pretreatment technology.

Research progress on emission and control of SO₃ and mercury in oxy-fuel combustion flue gas

Shiyao LIU Jiayu HUANG Jinhong LUO Shuang DENG Fengyan GUO

Chin. J. Process Eng.. 2019, 19(S1):  115-122.  DOI: 10.12034/j.issn.1009-606X.219176

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Oxy-fuel combustion technology, an effective greenhouse gas emission control technology, is an energy conservation and emission reduction technology with potential application. In this work the effects of flue gas components (SOx, NOx, H2O, Cl2/HCl etc.) on the formation of SO3 and Hg under oxy-fuel combustion condition, and the effects of fly ash on the adsorption and removal of SO3 and Hg enrichment in flue gas were systematically summarized and analysed. The feasible technical suggestions for synergistic control of SO3 and Hg under oxy-fuel combustion were put forward, which provides an important reference for the synergistic control of pollutants in the industrial application of oxy-fuel combustion. At the same time, the emission characteristics of SO3 and Hg under the current oxy-fuel combustion and the existing problems in the research direction of optimization control were analysed, and some suggestions for the future research direction were put forward.

Value-added utilization of crude glycerol from biodiesel production: catalytic oxydehydration to acrylic acid

Xiaona CHEN Dandan HE Zhipeng CHEN Licheng LIU

Chin. J. Process Eng.. 2019, 19(S1):  123-128.  DOI: 10.12034/j.issn.1009-606X.219196

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Since the biodiesel boom in the past ten years, glycerol became considerable oversupply in the market, as the main byproduct in biodiesel production through transesterification process. As a result, in recent years there have been intensive efforts devoted to convert glycerol to other value-added chemicals. The selective catalytic oxydehydration of glycerol to acrylic acid is an efficient way for value-added utilization of crude glycerol from biodiesel production. It couples glycerol dehydration to acrolein and acrolein oxidation to acrylic acid. Acrylic acid is a key feedstock for commodity acrylate esters and various functional polymers. This process allows producing acrylic acid from low-cost and renewable biomass resources instead of traditional crude oil feedstock. For developing this novel process, both catalyst (dehydration and oxidation) and technology are crucial in improving acrylic acid. In this study, some solid acid catalysts, such as Cs3PW12O40, P-ZSM-5 and Co0.5H2PO4/SiO2 were found to show high acrolein yield in glycerol dehydration at 300℃. The acrolein yield increased from 60.4% to 77.7% with respect to carrier gas (N2) flow rate on the Cs3PW12O40 catalyst. The acrolein yield went down from 75.0% to 65.8% when increasing P concentration from 2wt% to 20wt% over the phosphorous modified ZSM-5 catalysts. The 30wt% Co0.5H2PO4/SiO2 catalyst also showed excellent activity in dehydration of glycerol to acrolein. Nearly 80% of acrolein yield was obtained under 20 mL/min N2 flow rate. Interestingly, the acrolein yield increased to 86.9% when changing carrier gas to 20vol% O2/N2 with 25 mL/min flow rate. Using these catalysts and MoVW-based oxidation catalyst, the acrylic acid could be produced from glycerol with yield of 50%~80% with a dehydration/oxidation double catalyst bed configuration in one reactor at the same reaction temperature. Similar acrylic acid yield was obtained when feeding crude glycerol directly. The acetic acid and CO/CO2 were the main by-products for both reactions. The addition of methanol, NaCl, or NaOH to the glycerol feeding solution would reduce the acrolein yield for glycerol dehydration reaction. These additives are the general impurities in crude glycerol sample.