钙基高温二氧化碳吸附材料的制备及其吸附性能
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摘要
C02等温室气体的过量排放,是造成全球气候变化的主要原因之一。C02是主要的温室气体,控制和减少工业生产过程中的CO2排放对防止气候系统受到灾难性破坏具有重要意义。高温吸附捕集燃煤电厂烟道气中的CO2以及C02高温吸附强化甲烷水蒸汽重整等制氢过程,是CO2减排的有效途径,而且具有可观的经济效益。CaO吸附材料制备原料来源广泛且廉价、吸附容量高,是近期高温C02吸附剂的研究热点。但在高温C02吸附／解吸循环过程中,CaO吸附剂烧结失活,CO2吸附容量随着循环次数的增加而不断降低,对循环稳定性造成影响。本文的研究重点在于提高CaO吸附剂的循环稳定性和吸附容量,制备具有高吸附性能和抗烧结的新型钙基C02复合吸附材料,以满足高温C02吸附技术的应用需求。
本文首先采用天然钙源(扇贝壳、牡蛎壳、石灰石和白云石)、合成无机钙源(沉淀碳酸钙)、有机钙源(一水乙酸钙、四水柠檬酸钙和一水D葡萄糖酸钙)为原料,直接煅烧制备氧化钙吸附材料。考察了各氧化钙材料的CO2吸附性能与抗烧结性能。对失活氧化钙进行了水合活化再生研究,考察了水合活化再生对氧化钙材料形貌结构、C02吸附性能的影响。综合比较了不同钙源制备氧化钙的CO2吸附性能与成本,对制备钙回路捕集CO2吸附材料的可行性进行了分析讨论。
以沉淀碳酸钙、硝酸铝、硝酸镁、柠檬酸为原料,通过液相混合与阶段升温煅烧法分别制备了二元CaO-Al2O3和Ca-MgO钙基材料,以及三元CaO-Al2O3-MgO钙基复合材料。考察了添加A1203和添加MgO对二元及三元钙基材料的循环C02吸附性能的影响,探讨了二元及三元钙基材料的循环吸附稳定性机理。研究表明,添加A1203,形成Ca3Al2O6隋性支撑骨架负载氧化钙晶粒,高温循环过程中,氧化钙晶粒附着在骨架之上生长聚集,避免氧化钙晶粒大面积熔融烧结的发生,提高材料的循环吸附／解吸稳定性；而添加MgO,可促进CaO碳酸化反应,但对提高循环稳定性没有明显作用。三元钙基材料,物相组成为CaO、Ca3Al206和Mg0,可通过改变Ca3Al206和MgO的配比来调节材料的C02吸附容量和稳定性,对氧化钙含量低、循环稳定性高的材料,增加MgO的添加比例,不仅不会降低循环稳定性,还可以有效提高材料的CaO利用率,达到更高的C02吸附容量。
对C02吸附容量较高的二元及三元复合钙基材料进行长周期循环实验与钙回路C02捕获效率估算,结果显示,采用CaO-Al2O3和CaO-Al2O3-MgO钙基材料高温吸附捕集CO2,可大幅降低钙回路新鲜钙基吸附材料补充流量,具有较好的高温吸附捕集CO2应用前景。
Excessive emissions of greenhouse gases from the industrial processes are widely considered one of the main causes of global climate change. Carbon dioxide isan important greenhouse gas, andcarbon emission reduction is significant to prevent devastating damage with the climate system. High-temperature CO2adsorption technology is a cost-effective way to reduce CO2emissions directly from flue gases in power plants and from hydrogen preparation process by methane-steam reforming et al. Calcium based sorbent is a promising high-temperature CO2adsorbent material, since it has the advantages of lower preparation cost and higher CO2adsorption capacity. However, the rapid deactivation of calcium based sorbent due to sintering will reduce the CO2capture ability and lose the stability of sorbent during the multicyclic adsorption-desorption processes. This thesis will focus on the preparation of novel calcium based sorbents to improve the multicyclic adsorption/desorption stability and CO2capture ability at high temperature.
Calcium oxide sorbents are prepared by directly calcining some raw materials, including oyster shell, scallop shell, limestone. precipitated calcium carbonate, calcium acetate monohydrate, calcium citrate tetrahydrate. and calcium d-gluconate monohydrate. The CO2capture performance and anti-sintering behavior of the prepared CaO materials are investigated. The deactivated lime sorbents are reactivated through hydration, and the effects of hydration reactivation on CO2capture performance, morphologies and microstructure of lime sorbents are studied. The practicability of the prepared CaO materials in calcium looping CO2capture is evaluated through comparing the CO2capture performance and the preparation cost of sorbents.
Binary CaO-Al2O3and CaO-MgO sorbents. ternary CaO-Al2O3-MgO sorbent, are prepared through the liquid mixing reaction and following a four-step calcination method, where the precipitated calcium carbonate. aluminum nitrate, magnesium nitrate, and citric acid are used as raw materials. Effects of dopants (Al2O3and MgO) on the cyclic CO2capture performance of the prepared calcium-based sorbents are studied, and the anti-sintering mechanisms of three kinds of calcium based materials are analyzed and discussed. The results show that Al2O3doping can improve the cyclic CO2adsorption/desorption stability due to the formation of the inert supporting Ca3Al2O6framework, MgO doping can promote CaO carbonation reaction rate. By analysis of the microstructure of binary CaO-Al2O3material after many cycles, it is found that CaO grains are loaded on the inert supporting Ca3Al2O6framework. and grow and move on the Ca3Al2O6framework. thereby avoiding the sintering of material in a large range. Ternary CaO-Al2O3-MgO sorbent is composed of CaO. Ca3Al2O6and MgO. CO2capture ability and stability can be regulated by changing the mass ratio of Ca3Al2O6to MgO. For the ternary sorbent with high stability but low CO2capture ability due to low CaO content, the CO2capture ability can he improved by increasing the content of MgO without deteration of stability.
Long-term CO2adsorption/desorption cyclic tests are performed using CaO-Al2O3CaO-MgO, CaO-Al2O3-MgO and CaO sorbents, and the CO2capture abilities and CO2capture efficiencies in calcium looping process are estimated. The results show that, both CaO-Al2O3and CaO-Al2O3-MgO sorbents can effectively reduce the make-up flow of fresh sorbent, when compared with calcium oxide sorbent prepared by precipitated calcium carbonate. The prepared CaO-Al2O3and CaO-Al2O3-MgO materials in this thesis should have good industrial application prospect in the high-temperature CO2adsorption field.
本文首先采用天然钙源(扇贝壳、牡蛎壳、石灰石和白云石)、合成无机钙源(沉淀碳酸钙)、有机钙源(一水乙酸钙、四水柠檬酸钙和一水D葡萄糖酸钙)为原料,直接煅烧制备氧化钙吸附材料。考察了各氧化钙材料的CO2吸附性能与抗烧结性能。对失活氧化钙进行了水合活化再生研究,考察了水合活化再生对氧化钙材料形貌结构、C02吸附性能的影响。综合比较了不同钙源制备氧化钙的CO2吸附性能与成本,对制备钙回路捕集CO2吸附材料的可行性进行了分析讨论。
以沉淀碳酸钙、硝酸铝、硝酸镁、柠檬酸为原料,通过液相混合与阶段升温煅烧法分别制备了二元CaO-Al2O3和Ca-MgO钙基材料,以及三元CaO-Al2O3-MgO钙基复合材料。考察了添加A1203和添加MgO对二元及三元钙基材料的循环C02吸附性能的影响,探讨了二元及三元钙基材料的循环吸附稳定性机理。研究表明,添加A1203,形成Ca3Al2O6隋性支撑骨架负载氧化钙晶粒,高温循环过程中,氧化钙晶粒附着在骨架之上生长聚集,避免氧化钙晶粒大面积熔融烧结的发生,提高材料的循环吸附／解吸稳定性；而添加MgO,可促进CaO碳酸化反应,但对提高循环稳定性没有明显作用。三元钙基材料,物相组成为CaO、Ca3Al206和Mg0,可通过改变Ca3Al206和MgO的配比来调节材料的C02吸附容量和稳定性,对氧化钙含量低、循环稳定性高的材料,增加MgO的添加比例,不仅不会降低循环稳定性,还可以有效提高材料的CaO利用率,达到更高的C02吸附容量。
对C02吸附容量较高的二元及三元复合钙基材料进行长周期循环实验与钙回路C02捕获效率估算,结果显示,采用CaO-Al2O3和CaO-Al2O3-MgO钙基材料高温吸附捕集CO2,可大幅降低钙回路新鲜钙基吸附材料补充流量,具有较好的高温吸附捕集CO2应用前景。
Excessive emissions of greenhouse gases from the industrial processes are widely considered one of the main causes of global climate change. Carbon dioxide isan important greenhouse gas, andcarbon emission reduction is significant to prevent devastating damage with the climate system. High-temperature CO2adsorption technology is a cost-effective way to reduce CO2emissions directly from flue gases in power plants and from hydrogen preparation process by methane-steam reforming et al. Calcium based sorbent is a promising high-temperature CO2adsorbent material, since it has the advantages of lower preparation cost and higher CO2adsorption capacity. However, the rapid deactivation of calcium based sorbent due to sintering will reduce the CO2capture ability and lose the stability of sorbent during the multicyclic adsorption-desorption processes. This thesis will focus on the preparation of novel calcium based sorbents to improve the multicyclic adsorption/desorption stability and CO2capture ability at high temperature.
Calcium oxide sorbents are prepared by directly calcining some raw materials, including oyster shell, scallop shell, limestone. precipitated calcium carbonate, calcium acetate monohydrate, calcium citrate tetrahydrate. and calcium d-gluconate monohydrate. The CO2capture performance and anti-sintering behavior of the prepared CaO materials are investigated. The deactivated lime sorbents are reactivated through hydration, and the effects of hydration reactivation on CO2capture performance, morphologies and microstructure of lime sorbents are studied. The practicability of the prepared CaO materials in calcium looping CO2capture is evaluated through comparing the CO2capture performance and the preparation cost of sorbents.
Binary CaO-Al2O3and CaO-MgO sorbents. ternary CaO-Al2O3-MgO sorbent, are prepared through the liquid mixing reaction and following a four-step calcination method, where the precipitated calcium carbonate. aluminum nitrate, magnesium nitrate, and citric acid are used as raw materials. Effects of dopants (Al2O3and MgO) on the cyclic CO2capture performance of the prepared calcium-based sorbents are studied, and the anti-sintering mechanisms of three kinds of calcium based materials are analyzed and discussed. The results show that Al2O3doping can improve the cyclic CO2adsorption/desorption stability due to the formation of the inert supporting Ca3Al2O6framework, MgO doping can promote CaO carbonation reaction rate. By analysis of the microstructure of binary CaO-Al2O3material after many cycles, it is found that CaO grains are loaded on the inert supporting Ca3Al2O6framework. and grow and move on the Ca3Al2O6framework. thereby avoiding the sintering of material in a large range. Ternary CaO-Al2O3-MgO sorbent is composed of CaO. Ca3Al2O6and MgO. CO2capture ability and stability can be regulated by changing the mass ratio of Ca3Al2O6to MgO. For the ternary sorbent with high stability but low CO2capture ability due to low CaO content, the CO2capture ability can he improved by increasing the content of MgO without deteration of stability.
Long-term CO2adsorption/desorption cyclic tests are performed using CaO-Al2O3CaO-MgO, CaO-Al2O3-MgO and CaO sorbents, and the CO2capture abilities and CO2capture efficiencies in calcium looping process are estimated. The results show that, both CaO-Al2O3and CaO-Al2O3-MgO sorbents can effectively reduce the make-up flow of fresh sorbent, when compared with calcium oxide sorbent prepared by precipitated calcium carbonate. The prepared CaO-Al2O3and CaO-Al2O3-MgO materials in this thesis should have good industrial application prospect in the high-temperature CO2adsorption field.
引文
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