Change in the Pore Structure of Carbon-Carbon Composites during Successive Stages of High-Pressure Impregnation and Heat Treatment

Pore structure of C/C （Carbon-Carbon） composite after several stages of pitch impregnation under the high pressure and heat treatment was investigated by means of low temperature nitrogen adsorption and the standard contact porosimetry. Total pore volume, pore size distribution and specific surface area were calculated for samples of composite after several successive stages of treatment. The radius of pores presented in the material changes from 1 nm to 90 tam. Total pore volume and specific surface area both decrease after successive stages of pitch impregnation under the pressure, whereas heat treatment up to 1,750 ℃ and 2,000 ℃ leads to creation of some porous space and pore volume expansion. The bulk porosity of C/C composite comes down from 33.7% to 13.7% after the serial stages of treatment and the specific surface area is reduced by half compared to the initial material.

Effects of ultrasound on the desulfurization performance of hot coal gas over Zn-Mn-Cu supported on semi-coke sorbent prepared by high-pressure impregnation method

Zn-Mn-Cu/SC（U） sorbent was hydrothermally synthesized by ultrasound-assisted high-pressure impregnation method with semi-coke（SC）as support and the mixed solution of zinc nitrate,manganese nitrate and copper nitrate as active component precursors.The desulfurization performances of hot coal gas on the prepared sorbent at a mid-temperature of 500°C were tested in fixed-bed reactor.Morphology and pore structure of the prepared sorbent were also characterized by TEM,N2adsorption/desorption isotherms and XRD.For comparison,the sorbent of Zn-Mn-Cu/SC prepared by conventional high-pressure impregnation was also evaluated and characterized in order to study the effects of ultrasound treatment.Zn-Mn-Cu/SC（U） sorbent prepared by high-pressure impregnation under ultrasound-assisted condition showed a better desulfurization performance than Zn-Mn-Cu/SC.It could remove H2 S from 1000×10-6m3/m3 to 0.1×10-6m3/m3 at 500°C and maintained for 12.5 h with the sulfur capacity of 7.74%,in which both the breakthrough time and sulfur capacity were about 32% and 51% higher than those of Zn-Mn-Cu/SC sorbent.The introduction of ultrasound during high-pressure impregnation process greatly improved the morphology and pore structure of the sorbent.The ultrasonic treatment made particle size of active components smaller and made them more evenly disperse on semi-coke support,which provided more opportunities to contact with H2S in coal-based gases.However,there were no any difference in compositions and existing forms of active components on the Zn-Mn-Cu/SC and Zn-Mn-Cu/SC（U） sorbents.

INFLUENCE OF HEAT TREATMENT ON OXIDATION PROPERTIES OF C/C COMPOSITES FABRICATED BY HIGH PRESSURE IMPREGNATION CARBONIZATION

Felt base carbon/carbon composites fabricated by super-high pressure impregnation carbonization process (SPIC) were heat treated at high temperature 2773K. The oxidation properties of felt base carbon/carbon composites were investigated at different temperatures (773-1173K), and the microstructures of carbon/carbon composites were studied by SEM and X-ray diffraction. The experimental results showed that the inter-laminar distance of (002) plane (d002) deceased while the microcrystalline stack height (Lc) increased. The oxidation rate of felt base carbon/carbon composites was invari-able at certain temperatures. The oxidation mechanism of carbon/carbon composites changed remarkably at the oxidation temperature 973K. At the initial oxidation stage of carbon/carbon composites, carbon matrix was oxidized much more rapidly than carbon felt.

Lignocellulosic-Based Activated Carbon Prepared by a Chemical Impregnation Method as Electrode Materials for Double Layer Capacitor

Activated carbons (ACs) were prepared from a lignocellulosic-based waste material by a chemical impregnation method using KOH, NaOH or CaCl2 as the activating agent. These ACs were characterized by different techniques such as N2 adsorption, FTIR, XRD and SEM. Electrostatic properties viz. pH and pHpzc of AC suspensions in aqueous media were measured. The concentration of surface oxygenated functional groups of the ACs was estimated following the Boehm titration method. Cyclic voltammetry was conducted in H2SO4 after fabricating two-electrode capacitor cells of the ACs. The correlation of AC surface chemistry and morphology with electrochemical performance (capacitance) of powdered electrodes is analyzed and discussed.

Impregnation of Carbonate Rock with Bituminous Compounds. II. Improvement of the Impregnation Material

The steam-thermal method for refinery of highly-viscous oils and the process of propane-butane liquid extraction have been implemented for production of the impregnation material for carbon rock. The process of steam-thermal treatment has been carried out for highly-viscous oil from Ashalchinskoye accumulation with the “steam-oil” ratio changing from 1.1:1 to 1.4:1. The extraction process has been carried out at temperature T = 85°C and pressures from 4.5 to 8 MPa. Water absorption of carbonate rock has decreased to 0.34% as a result of SCF-impregnation process.

Effects of impregnation sequence on the microstructure and performances of Cu-Co based catalysts for the synthesis of higher alcohols

Silica-supported CuCo catalysts were prepared by impregnation method with different impregnation sequence for higher alcohols synthesis. These catalysts were characterized by H2-TPR, XRD, N2 adsorption, XPS techniques and CO selective hydrogenation reaction measurement. The effects of impregnation sequence on the structure and performance of catalysts were investigated, and there were important influences on the selectivity to higher alcohols. There was a strong synergistic effect between copper and cobalt for the co-impregnated sample. The CuCo/SiO2 catalyst prepared by co- impregnation showed a better yield of total alcohols, and a higher selectivity to total alcohols which reached 51.5%.

High-pressure capacity expansion and water injection mechanism and indicator curve model for fractured-vuggy carbonate reservoirs

Water injection for oil displacement is one of the most effective ways to develop fractured-vuggy carbonate reservoirs.With the increase in the number of rounds of water injection,the development effect gradually fails.The emergence of high-pressure capacity expansion and water injection technology allows increased production from old wells.Although high-pressure capacity expansion and water injection technology has been implemented in practice for nearly 10 years in fractured-vuggy reservoirs,its mechanism remains unclear,and the water injection curve is not apparent.In the past,evaluating its effect could only be done by measuring the injection-production volume.In this study,we analyze the mechanism of high-pressure capacity expansion and water injection.We propose a fluid exchange index for high-pressure capacity expansion and water injection and establish a discrete model suitable for high-pressure capacity expansion and water injection curves in fractured-vuggy reservoirs.We propose the following mechanisms:replenishing energy,increasing energy,replacing energy,and releasing energy.The above mechanisms can be identified by the high-pressure capacity expansion and water injection curve of the well HA6X in the Halahatang Oilfield in the Tarim Basin.By solving the basic model,the relative errors of Reservoirs I and II are found to be 1.9%and 1.5%,respectively,and the application of field examples demonstrates that our proposed high-pressure capacity expansion and water injection indicator curve is reasonable and reliable.This research can provide theoretical support for high-pressure capacity expansion and water injection technology in fracture-vuggy carbonate reservoirs.

Impact of impregnation pressure on desulfurization performance of Zn-based sorbents supported on semi-coke

High-pressure impregnation, a new preparation method for sorbents to remove H2S from hot coal gas, is introduced in this paper. Semi-coke （SC） and ZnO is selected as the support and active component of sorbent, respectively. The sorbent preparation process includes high-pressure impregnation, filtration, ovendry and calcination. The aim of this research is to primarily study the effects of the impregnation pressure on physical properties and desulfurization ability of the sorbent. The desulfurization experiment was carried out in a fixed-bed reactor at 500 ~C and a simulated coal gas used in this work was composed of CO （33 vol%）, H2 （39 vol%）, H2S （300 ppm in volume）, and N2 （balance）. Experimental results show that the pore structure of the SC support can be improved effectively and ZnO active component can be uniformly dispersed on the support, with the small particle size of 10-500 nm. Sorbents prepared using high-pressure impregnation have better desulfurization capacity and their active components have higher utilization rate. P20-ZnSC sorbent, obtained by high-pressure impregnation at 20 atm, has the best desulfurization ability with a sulfur capacity of 7.54 g S/100g sorbent and a breakthrough time of 44 h. Its desulfurization precision and efficiency of removing H2S from the middle temperature gases can reach 〈 1 ppm and 〉99.7%, respectively, before sorbent breakthrough.

Impregnation of Crushed Stone with Bitumenous Compounds Using Propane/Butane Impregnation Process Carried out in Supercritical Fluid Conditions

An efficient technology of impregnation of carbonate crushed stone by oil-product based on SCF-impregnation process usage with propane/butane solvent was developed. Regular impregnation throughout the volume of crushed stone sample is achieved. As a result of the appliance of proposed technology, the humidity of the treated crushed stone samples decreased down to 0.54%.

Removal of CO2 in a multistage fluidized bed reactor by amine impregnated activated carbon: optimization using response surface methodology

Carbon dioxide (CO2) is the major component of greenhouse gas. Increase in concentration of CO2 in the atmosphere leads to global warming. To remove the CO2 from waste flue gas a four-stage counter-current multistage fluidized bed adsorber was developed and operated in continuous bubbling fluidization regime for the two丒phase system. This paper describes the optimum condition for CO2 removal efficiency in a multistage fluidized bed reactor using amine impregnated activated carbon. Response surface methodology with central composite design was used to determine the effect of three variables on the response. The variables are inlet concentration of CO2 in ppm (ranging from 3000 to 20,000), impregnation ratio of monoethanol amine (ranging from 0.2 to 0.6) and weir height in mm (20-60). The response was CO2 removal efficiency. The factor which was most influential has been identified from the analysis of variance. The optimum CO2 removal efficiency for the amine impregnated activated carbon (MEA-AC) was found to be 95.17%, at initial concentration of CO2 7312.85 ppm, chemical impregnation ratio of 0.31, and weir height 48.65 mm. From the experiment, the CO2 removal efficiency was found to be 95.97% at the same operating conditions. The predicted response was found to relevance with experimental data.

ANALYSIS OF THE REMOVAL OF H_2S WITH IMPREGNATED ACTIVATED CARBON

A general mathematical model with its governing equations in dimensionless forms has beendeveloped to describe the removal of hydrogen sulfide with impregnated activated carbon.Anapproximate relationship between the sulfur capacity and the reaction time in a single carbon pellet isobtained,and criterion to ascertain the rate controlling step of the process can then be deduced.Inthe meantime,the choice of the appropriate oxygen concentration and the principle to be followedare also described.

Mechanism, behaviour and application of iron nitrate modified carbon nanotube composites for the adsorption of arsenic in aqueous solutions

In this study,ferric nitrate modified carbon nanotube composites (FCNT) were prepared by isovolumetric impregnation using carbon nanotubes (CNTs) as the carrier and ferric nitrates the active agent.The batch experiments showed that FCNT could effectively oxidize As(III) to As(V) and react with it to form stable iron arsenate precipitates.When the dosage of FCNT was 0.1 g·L^(–1),pH value was 5–6,reaction temperature was 35℃ and reaction time was 2 h,the best arsenic removal effect could be achieved,and the removal rate of As(V) could reach 99.1%,which was always higher than 90%under acidic conditions.The adsorption results of FCNT were found to be consistent with Langmuir adsorption by static adsorption isotherm fitting,and the maximum adsorption capacity reached 118.3 mg·g^(-1).The material phase and property analysis by scanning electron microscopy,Brunauer–Emmett–Teller,Fourier transform infrared spectoscopy,X-ray photoelectron spectroscopy and other characterization methods,as well as adsorption isotherm modeling,were used to explore the adsorption mechanism of FCNT on arsenic.It was found that FCNT has microporous structure and nanostructure,and iron nanoparticles are loosely distributed on CNTs,which makes the material have good oxidation,adsorption and magnetic separation properties.Arsenic migrates on the surface of FCNT composites is mainly removed by forming insoluble compounds and co-precipitation.All the results show that FCNT treats arsenic at low cost with high adsorption efficiency,and the results also provide the experimental data basis and theoretical basis for arsenic contamination in groundwater.

Preparation of activated carbon from sunflower straw through H_(3)PO_(4) activation and its application for acid fuchsin dye adsorption

With the development circular economy, the use of agricultural waste to prepare biomass materials to remove pollutants has become a research hotspot. In this study, sunflower straw activated carbon (SSAC) was prepared by the one-step activation method, with sunflower straw (SS) used as the raw material and H3PO4 used as the activator. Four types of SSAC were prepared with impregnation ratios (weight of SS to weight of H3PO4) of 1:1, 1:2, 1:3, and 1:5, corresponding to SSAC1, SSAC2, SSAC3, and SSAC4, respectively. The adsorption process of acid fuchsin (AF) in water using the four types of SSAC was studied. The results showed that the impregnation ratio significantly affected the structure of the materials. The increase in the impregnation ratio increased the specific surface area and pore volume of SSAC and improved the adsorption capacity of AF. However, an impregnation ratio that was too large led to a decrease in specific surface area. SSAC3, with an impregnation ratio of 1:3, had the largest specific surface area (1 794.01 m2/g), and SSAC4, with an impregnation ratio of 1:5, exhibited the smallest microporosity (0.052 7 cm3/g) and the largest pore volume (2.549 cm3/g). The adsorption kinetics of AF using the four types of SSAC agreed with the quasi-second-order adsorption kinetic model. The Langmuir isotherm model was suitable to describe SSAC3 and SSAC4, and the Freundlich isotherm model was appropriate to describe SSAC1 and SSAC2. The result of thermodynamics showed that the adsorption process was spontaneous and endothermic. At 303 K, SSAC4 showed a removal rate of 97.73% for 200-mg/L AF with a maximum adsorption capacity of 2 763.36 mg/g, the highest among the four types of SSAC. This study showed that SAAC prepared by the H3PO4-based one-step activation method is a green and efficient carbon material and has significant application potential for the treatment of dye-containing wastewater.

Synthesis of the Palladium Catalyst with the Supercritical СO2-Impregnation Method Realized in the Static Mode

Results of research of supercritical fluid CO2-impregnation process (the static mode) within a problem of synthesis of the palladium catalyst are given. The kinetics of process is characterized in the pressure range from 15.0 to 35.0 MPa on temperatures 308.15?K, 313.15?K, 318.15?K, 323.15?K, 328.15?K and 333.15?K. Results of surface assessment and activity measurements of the catalyst samples synthesized by supercritical СO2-impregnation of aluminum oxide suggest competitiveness of the discussed approach in comparison to traditional methods.

Supercritical Fluid Impregnation of Essential Bark Oil in Copolymers of L-Lactide with 7-Membered Cyclic Compounds

In order to develop a novel controlled-release material, we previously attempted to impregnate poly(L-lactide) (poly(L-LA)), poly(L-LA-ran-CL) (CL: ε-caprolactone) or poly(L-LA-ran-TEMC) (TEMC: tetramethylene carbonate) with low boiling point, organic useful compounds using supercritical carbon dioxide (scCO2) as the solvent. In this work, the factors influencing impregnation of poly (L-LA) random copolymers with useful compounds were investigated under scCO2 using the copolymers previously used. The influence of temperature, pressure, and time on the impregnation contents of the useful compounds on the copolymers was evaluated. The polymer used, which is a base of this material, was poly(L-LA-ran-CL), poly(L-LA-ran-TEMC), or poly(L-LA-ran-DXO) (DXO: 1,5-dioxepan-2-one). Statistical random copolymers of L-LA with CL, TEMC, or DXO were synthesized using Sn(oct)2 as a catalyst at 150°C for 24 h without solvent. Preparation of the controlled-release materials was carried out using essential bark oil from Thujopsis dolabrata var. hondae and synthetic L-LA random copolymers as a base material under scCO2. The impregnation experiment, which investigated the influence of pressure, was conducted in the range of 10 to 20 MPa. The influence of temperature on impregnation was carried out at 40°C to 100°C. Impregnation time was varied from 1 to 5 h. The pressure of essential oil impregnated into poly(L-LA) random copolymers was the highest at 14 MPa. In the influence of temperature on impregnation, the amount of essential oil increased with increasing temperature.

Preparation and Characterization of Stellera Chamaejasme-Based Carbon Molecular Sieves

The activation effect of boric acid as an activator is good,and we investigate the best activation conditions for the boric acid impregnation method.To represent the structural characteristics and adsorption performance of the Stellera Chamaejasme based carbon molecular sieves,we use Brunner-Emmet-Teller(BET)measurements,scan-ning electron microscope(SEM),Raman spectra(Raman),X-ray diffraction(XRD),and adsorption property measurement.When the loading ratio was 0.68:1,the specific surface area was 532.21 m^(2)/g,the total pore volume was 0.24 cm 3/g,the average pore size was 1.81 nm,the adsorption value of methylene blue was 145.28 mg/g,and the adsorption value of iodine was 713.33 mg/g,the results showed that boric acid had better activation effect.The carbon molecular sieves made from Stellera Chamaejasme and activated with boric acid produce two peaks on the aperture distribution graph that are densely distributed in the micropore range.This indicates that boric acid’s pore-forming tendency is primarily micropore.

预浸碳化再生骨料混凝土的动态力学性能研究

为研究再生骨料的预浸碳化处理方式及碳化循环次数对再生混凝土动态力学性能的影响,将强化后的再生骨料100%取代天然骨料制备再生混凝土试件,分别开展静、动态压缩试验。研究结果表明,静态加载时,预浸碳化组的抗压强度随碳化循环次数的增加而增大,而直接碳化组的抗压强度仅在第1次碳化循环后有所提升,继续进行碳化循环对再生混凝土强度的提升效果不明显。动态加载时,预浸碳化组再生混凝土呈现出明显的应变率强化效应,动态抗压强度与动态增加因子均随应变率的增大而提高,相较于普通再生混凝土,再生骨料预浸碳化循环3次后制备的再生混凝土试件动态抗压强度提升了23.8%,而直接碳化组仅提升了5.7%,且动态增加因子与应变率的对数存在良好的线性关系,随应变率的lg10线性增加;当应变率相同时,随着碳化循环次数的增加,动态抗压强度也增大。从能量的角度看,预浸碳化组在高应变率下的比能量吸收值大于低应变率下的比能量吸收值,再次说明了预浸碳化再生骨料混凝土仍具有应变率效应,相同应变率条件下,预浸碳化组的比能量吸收值大于直接碳化组,说明预浸碳化再生骨料提升了再生混凝土的抗冲击性能,且效果优于传统的直接碳化处理。上述研究也为预浸碳化强化再生骨料及再生混凝土在工程结构中的应用提供了可靠的试验结果和理论依据。

环境湿度对浸金属碳滑板磨损及温升的影响

为探究环境湿度对弓网摩擦副载流滑动过程中电弧放电能量、浸金属碳滑板温升及滑板磨损量的影响,采用环-块式高速载流摩擦磨损试验台,对比不同湿度条件下,电弧能量、滑板温升及滑板磨损量随滑动速度、电流强度、法向力的变化情况。试验结果表明:不同环境湿度下,滑动速度和电流强度的增大均会导致电弧能量及滑板温升急剧增大;电弧热是导致温升的主要热源;增大法向力对于抑制电弧放电、降低滑板温升均有显著效果,而对于滑板磨损量变化的影响,不同湿度情况则截然相反;高湿度环境下接触副附着的水膜改善了接触状况和散热情况,电弧能量及滑板温升都小于低湿度环境;低湿度环境下滑板表面受到更严重的机械摩擦,其表面状态相比高湿度更差;在平均湿度较高的夏季适当增加升弓压力,在平均湿度较低的冬季适当降低列车行驶速度可以减少浸金属碳滑板磨损。

浸渍活性炭吸附放射性碘甲烷后失活机理研究

核电站通风净化系统采用浸渍活性炭(IMAC)吸收核反应所产生的放射性气态碘,以确保环境及人员安全。IMAC长时间连续使用后吸附效率明显下降。明晰IMAC的失活机理,对延长其使用寿命及后续高值化利用研究意义重大。选用基炭、浸渍活性炭、失活活性炭为研究对象,分析了其微观形貌和物相组成,探讨了IMAC失活前后的变化规律,推断其失活机理。结果表明:IMAC主要活性组分三乙烯二胺(TEDA)部分与碘甲烷发生反应生成四铵盐,且TEDA易分解,含量减少90%以上。环境中的氧化性物质和IMAC表面含氧官能团对活性炭造成不同程度的氧化,同时微孔比表面积占总比表面积由85%下降至40%以下,碘甲烷吸附场所减少。以上原因造成IMAC表面结构改变,活性位点减少,导致其吸附效率下降。

流化床喷雾浸渍制备负载型钠基CO_(2)吸附剂脱碳性能

针对传统钠基CO_(2)固体吸附剂晶粒尺寸大、气体扩散阻力高、负载量有限导致的吸附量低的瓶颈问题,提出了基于流化床喷雾浸渍技术的吸附剂制备新方法。选取γ-Al_(2)O_(3)为载体,高纯度Na_(2)CO_(3)作为活性组分,利用溶液浸渍法和流化床喷雾浸渍法分别制备了载体结构、活性组分负载量不同的多组吸附剂,并基于固定床实验装置结合比表面积和孔隙度分析仪、X射线衍射仪、扫描电子显微镜、X射线荧光光谱分析等手段对吸附剂的CO_(2)吸附性能以及孔隙结构、晶型、表面形态及负载量等关键参数进行表征。研究结果表明,相同活性组分负载量下,采用喷雾浸渍法制备的吸附剂的饱和吸附量和吸附活性皆优于传统浸渍法,其原因在于该方法可以控制活性组分在载体上的负载深度;同时,活性组分多为针状或棒状等利于反应的形态结晶;晶体尺寸较传统溶液浸渍法普遍小10%~20%。尽管如此,载体的孔隙结构,具体如比表面积和孔径分布等参数仍会限制流化床喷雾浸渍技术制备的吸附剂的反应性能。