CN101269320A - Preparation method of calcium-based carbon dioxide adsorbent - Google Patents
Preparation method of calcium-based carbon dioxide adsorbent Download PDFInfo
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000011575 calcium Substances 0.000 title claims abstract description 49
- 229910052791 calcium Inorganic materials 0.000 title claims abstract description 47
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000003463 adsorbent Substances 0.000 title claims description 58
- 229910002092 carbon dioxide Inorganic materials 0.000 title abstract description 20
- 239000001569 carbon dioxide Substances 0.000 title abstract description 5
- 239000002351 wastewater Substances 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000012265 solid product Substances 0.000 claims abstract description 4
- 235000019738 Limestone Nutrition 0.000 claims description 10
- 239000000292 calcium oxide Substances 0.000 claims description 10
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 10
- 239000006028 limestone Substances 0.000 claims description 10
- 238000001179 sorption measurement Methods 0.000 claims description 8
- 239000010459 dolomite Substances 0.000 claims description 7
- 229910000514 dolomite Inorganic materials 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 4
- 239000003814 drug Substances 0.000 claims description 2
- 239000000975 dye Substances 0.000 claims description 2
- 235000013305 food Nutrition 0.000 claims description 2
- 235000013599 spices Nutrition 0.000 claims description 2
- 239000004753 textile Substances 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 9
- 229960004424 carbon dioxide Drugs 0.000 claims 4
- 235000011089 carbon dioxide Nutrition 0.000 claims 4
- 239000000047 product Substances 0.000 claims 2
- 239000003905 agrochemical Substances 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 123
- 238000001354 calcination Methods 0.000 abstract description 20
- 125000004122 cyclic group Chemical group 0.000 abstract description 16
- 239000002594 sorbent Substances 0.000 abstract description 9
- 239000007795 chemical reaction product Substances 0.000 abstract description 6
- 238000002485 combustion reaction Methods 0.000 abstract description 6
- 238000002309 gasification Methods 0.000 abstract description 4
- 239000002028 Biomass Substances 0.000 abstract description 2
- 238000003763 carbonization Methods 0.000 abstract description 2
- 239000013064 chemical raw material Substances 0.000 abstract description 2
- 239000002803 fossil fuel Substances 0.000 abstract description 2
- 230000001143 conditioned effect Effects 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000003750 conditioning effect Effects 0.000 description 12
- 239000011148 porous material Substances 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
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- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 150000001669 calcium Chemical class 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
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- -1 stir while adding Substances 0.000 description 1
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Abstract
Description
技术领域 technical field
本发明涉及增强钙基吸附剂循环捕捉CO2性能的方法，属于环境污染防治与洁净煤燃烧技术领域。The invention relates to a method for enhancing the performance of a calcium-based adsorbent for cyclically capturing CO2 , and belongs to the technical fields of environmental pollution prevention and clean coal combustion.
背景技术 Background technique
目前，以CO2为主的温室气体所引起的全球变暖已受到世界各国的普遍关注。2004年美国公布的数据显示，从2000年到2004年全球CO2排放水平每年增加3％——这一速度是1990年到1999年CO2排放增加速度(1.1％)的近3倍。这将会引发植被的迁徙与物种灭绝，气候带移动，海平面上升与陆地淹没，洋流变化与厄尔尼诺频发等现象。我国是CO2排放大国，尤其是燃煤电站CO2的排放控制已经到了刻不容缓的地步。At present, global warming caused by CO 2 -based greenhouse gases has drawn widespread attention from all over the world. According to data released by the United States in 2004, the level of global CO 2 emissions increased by 3% per year from 2000 to 2004—a rate nearly three times that of the increase in CO 2 emissions (1.1%) from 1990 to 1999. This will lead to the migration of vegetation and species extinction, the movement of climate zones, sea level rise and land submersion, changes in ocean currents and frequent occurrence of El Niño, etc. China is a big CO 2 emission country, especially the CO 2 emission control of coal-fired power plants has reached the point of no delay.
CO2控制方法众多，这些方法中既包括物理分离法，如膜分离法，也包括化学吸附法，如胺吸收法、生物吸收法和化学链燃烧法等。一般认为化学吸附法具有更高的CO2脱除效率，然而技术经济性也是选择CO2减排方式的重要因素，大规模减排CO2方式对于技术经济性提出了更高的要求。选择廉价高效的CO2吸附剂是有效控制CO2排放的关键。近年来，钙基吸附剂的煅烧/碳酸化反应分离CO2的方法引起了各国学者的极大兴趣和广泛关注。该方法采用价格低廉、分布广泛的石灰石和白云石作为CO2吸附剂。钙基吸附剂循环煅烧/碳酸化反应，既可以在美国Los Alamos国家实验室提出的以煤直接制氢为核心的近零排放煤炭发电技术中分离CO2，也可以在加拿大能源矿产中心(CANMET)提出的双流化床煤燃烧系统中床内直接捕捉CO2。There are many methods for CO2 control, including physical separation methods, such as membrane separation methods, and chemical adsorption methods, such as amine absorption methods, biological absorption methods, and chemical looping combustion methods. It is generally believed that the chemical adsorption method has a higher CO 2 removal efficiency, but the technical economy is also an important factor in choosing a CO 2 emission reduction method, and the large-scale CO 2 emission reduction method puts forward higher requirements for the technical economy. The selection of cheap and efficient CO2 adsorbents is the key to effectively control CO2 emissions. In recent years, the method of calcination/carbonation reaction of calcium-based adsorbents to separate CO2 has attracted great interest and widespread attention from scholars from various countries. The method employs inexpensive and widely distributed limestone and dolomite as CO2 adsorbents. The cyclic calcination/carbonation reaction of calcium-based adsorbents can separate CO 2 in the near-zero-emission coal power generation technology proposed by the Los Alamos National Laboratory in the United States, which focuses on direct hydrogen production from coal, and can also be used in the Canadian Center for Energy and Minerals (CANMET ) in the double fluidized bed coal combustion system to directly capture CO 2 in the bed.
以化石燃料、生物质燃烧或气化过程中钙基吸附剂如石灰石循环煅烧/碳酸化捕捉CO2系统为例进行说明。如图1所示，钙基吸附剂进入煅烧炉，该炉内采用O2/CO2循环燃烧方式提供钙基吸附剂分解所需的热量，使分解的CO2便于回收，形成的CaO进入到碳酸化反应器中捕捉燃烧或气化反应产生的CO2，形成的碳酸钙再到煅烧炉中分解再生为CaO，反应循环进行。失活的CaO被排出，同时添加新鲜的吸附剂以补充失活的吸附剂。然而钙基吸附剂在循环煅烧/碳酸化反应中存在一个明显的不足：即随着循环反应次数的增加，碳酸化性能即捕捉CO2的能力迅速下降。为了保持较高的CO2脱除效率，不得不额外补充大量新鲜吸附剂。大量的钙基吸附剂在反应器内循环不仅使运行成本增加，而且还能使反应器的磨损、粘污和腐蚀加剧。因此提高钙基吸附剂循环吸附CO2的能力，以较少的钙基吸附剂取得较高的CO2循环脱除能力对于安全经济运行具有十分重要的意义和价值。The system for CO2 capture by cyclic calcination/carbonation of calcium-based adsorbents such as limestone during fossil fuel, biomass combustion or gasification process is illustrated as an example. As shown in Figure 1, the calcium-based adsorbent enters the calciner, and the O 2 /CO 2 cycle combustion method is adopted in the furnace to provide the heat required for the decomposition of the calcium-based adsorbent, so that the decomposed CO 2 is easy to recover, and the formed CaO enters the CO 2 produced by combustion or gasification is captured in the carbonation reactor, and the formed calcium carbonate is decomposed and regenerated into CaO in the calciner, and the reaction cycle is carried out. The deactivated CaO is expelled while adding fresh sorbent to replenish the deactivated sorbent. However, there is an obvious shortcoming of calcium-based adsorbents in cyclic calcination/carbonation reactions: that is, the carbonation performance, that is, the ability to capture CO 2 , decreases rapidly as the number of cyclic reactions increases. In order to maintain a high CO2 removal efficiency, a large amount of fresh adsorbent has to be replenished additionally. The circulation of a large amount of calcium-based adsorbent in the reactor not only increases the operating cost, but also aggravates the wear, fouling and corrosion of the reactor. Therefore, it is of great significance and value to improve the ability of calcium-based adsorbents to adsorb CO 2 in a cycle and to obtain a higher cycle removal capacity of CO 2 with less calcium-based adsorbents for safe and economical operation.
发明内容 Contents of the invention
技术问题：本发明的目的是提供一种既能提高钙基吸附剂循环捕捉CO2性能，又能处理乙酸废水的钙基二氧化碳吸附剂的制备方法。该方法不仅能有效抑制随循环反应次数增加钙基吸附剂碳酸化转化率的严重衰减，增加吸附剂在循环反应过程中的抗烧结性能，减小新鲜吸附剂的添加量，减轻反应设备的磨损和腐蚀，而且能够处理乙酸废水中的乙酸和回收丙酮。Technical problem: The purpose of the present invention is to provide a preparation method of a calcium-based carbon dioxide adsorbent that can not only improve the performance of the calcium-based adsorbent to capture CO2 in circulation, but also treat acetic acid wastewater. This method can not only effectively suppress the severe attenuation of the carbonation conversion rate of the calcium-based adsorbent as the number of cyclic reactions increases, but also increase the anti-sintering performance of the adsorbent during the cyclic reaction process, reduce the amount of fresh adsorbent added, and reduce the wear of the reaction equipment. and corrosion, and can treat acetic acid in acetic acid wastewater and recover acetone.
技术方案：在常温常压条件下，将乙酸废水置于容器内，将石灰石、白云石及氧化钙等钙基吸附剂颗粒加入乙酸废水中，边加入边搅拌，乙酸废水中乙酸与钙基吸附剂中Ca的摩尔比高于1.5∶1，在反应过程中保持搅拌使钙基吸附剂与乙酸废水反应均匀，反应5小时后，将容器内的反应产物进行加热干燥脱水。乙酸废水调质钙基吸附剂后得到的反应产物能释放出丙酮，采用干馏的方法可回收丙酮，剩余固体产物作为CO2吸附剂。乙酸废水是食品、或轻纺、或医药、或染料、或香料、或农药产生的乙酸废水，钙基吸附剂的原料是石灰石、或白云石、或氧化钙。Technical solution: Under normal temperature and pressure conditions, put acetic acid wastewater in a container, add calcium-based adsorbent particles such as limestone, dolomite and calcium oxide into the acetic acid wastewater, stir while adding, acetic acid and calcium-based adsorption in the acetic acid wastewater The molar ratio of Ca in the agent is higher than 1.5:1. Keep stirring during the reaction to make the calcium-based adsorbent and acetic acid wastewater react evenly. After 5 hours of reaction, the reaction product in the container is heated, dried and dehydrated. Acetone can be released from the reaction product obtained after conditioning the calcium-based adsorbent by acetic acid wastewater, and acetone can be recovered by dry distillation, and the remaining solid product is used as a CO2 adsorbent. Acetic acid wastewater is produced by food, or textile, or medicine, or dyes, or spices, or pesticides. The raw material of calcium-based adsorbent is limestone, or dolomite, or calcium oxide.
检测结果表明，经乙酸溶液调质后的钙基吸附剂第1次煅烧后CaO晶粒尺寸小于原钙基吸附剂第1次煅烧后的CaO晶粒尺寸。随着循环反应次数的增加，原钙基吸附剂煅烧后CaO的晶粒尺寸迅速变大，晶粒间的孔隙随之减小，从而增大了CO2在颗粒中的扩散阻力，对碳酸化反应是不利的；而经乙酸溶液调质后的吸附剂煅烧后随循环次数的增加，CaO晶粒尺寸增加缓慢，表现出了较强的抗烧结性能，较好地保持了晶粒间的孔隙，这有利于CO2在晶粒间的扩散。采用氮吸附仪对乙酸溶液调质前后吸附剂煅烧后的孔结构参数进行分析，结果表明，和原吸附剂的比表面积和比孔容随循环次数的增加迅速减小相比，乙酸溶液调质后的吸附剂煅烧后比表面积和比孔容均远高于原吸附剂，并且随着循环反应次数的增加比表面积和比孔容下降缓慢，在经相同循环反应次数后乙酸溶液调质后的吸附剂煅烧后孔分布更优于原吸附剂。由于乙酸溶液调质优化了钙基吸附剂煅烧后的微观结构，使得钙基吸附剂具有更为良好的碳酸化性能和抗烧结性能。The test results show that the CaO grain size of the calcium-based adsorbent after the first calcination after conditioning by acetic acid solution is smaller than the CaO grain size of the original calcium-based adsorbent after the first calcination. With the increase of the number of cyclic reactions, the grain size of CaO increases rapidly after the original calcium-based adsorbent is calcined, and the pores between the grains decrease accordingly, thereby increasing the diffusion resistance of CO2 in the particles and affecting carbonation. The reaction is unfavorable; however, the CaO grain size increases slowly with the increase of the number of cycles after calcination of the adsorbent tempered by acetic acid solution, which shows strong anti-sintering performance and better maintains the pores between the grains. , which facilitates the diffusion of CO2 between grains. A nitrogen adsorption instrument was used to analyze the pore structure parameters of the adsorbent after calcination before and after the conditioning of the acetic acid solution. The specific surface area and specific pore volume of the final adsorbent after calcination are much higher than that of the original adsorbent, and the specific surface area and specific pore volume decrease slowly with the increase of the number of cyclic reactions. The pore distribution after calcination is better than that of the original adsorbent. Because the acetic acid solution optimizes the microstructure of the calcined calcium-based adsorbent, the calcium-based adsorbent has better carbonation performance and anti-sintering performance.
有益效果：采用乙酸废水调质钙基吸附剂提高其循环捕捉CO2性能具有以下优点：Beneficial effects: Using acetic acid wastewater to condition calcium-based adsorbent to improve its performance of recycling CO2 capture has the following advantages:
1.明显提高了钙基吸附剂在长期循环煅烧/碳酸化过程中的抗烧结性能和循环捕捉CO2的能力。1. Significantly improved the anti-sintering performance of calcium-based adsorbents in the long-term cyclic calcination/carbonation process and the ability to capture CO 2 cyclically.
2.能够有效处理乙酸废水中的乙酸，减小乙酸废水排放所引起的环境污染。2. It can effectively treat the acetic acid in the acetic acid wastewater and reduce the environmental pollution caused by the discharge of the acetic acid wastewater.
3.可以从乙酸废水调质后的钙基吸附剂中回收丙酮，可作化工原料，提高了反应过程的经济性。3. The acetone can be recovered from the calcium-based adsorbent after conditioning by acetic acid wastewater, which can be used as a chemical raw material and improves the economy of the reaction process.
4.采用改性的钙基CO2吸附剂可以降低运行成本，在一定程度上可减轻碳酸化过程中钙基吸附剂对设备的磨蚀。4. The use of modified calcium-based CO2 adsorbents can reduce operating costs, and to a certain extent, reduce the abrasion of calcium-based adsorbents on equipment during the carbonation process.
附图说明 Description of drawings
图1为钙基吸附剂在燃烧或气化过程中以循环煅烧/碳酸化反应方式捕捉CO2流程图；Figure 1 is a flow chart of calcium-based adsorbents capturing CO in a cyclic calcination/carbonation reaction during combustion or gasification;
图2为在循环煅烧/碳酸化过程中采用乙酸废水调质钙基吸附剂的工艺流程图。Fig. 2 is a process flow diagram of using acetic acid wastewater to condition calcium-based adsorbents in the cyclic calcination/carbonation process.
具体实施方式 Detailed ways
图2为在循环煅烧/碳酸化过程中采用乙酸废水调质钙基吸附剂的工艺流程图。钙基吸附剂进入调质反应塔与乙酸废水发生酸化反应，调质后的吸附剂再进入干馏反应塔进行干馏，回收调质吸附剂释放出的丙酮，然后再进行煅烧/碳酸化反应循环捕捉CO2。Fig. 2 is a process flow diagram of using acetic acid wastewater to condition calcium-based adsorbents in the cyclic calcination/carbonation process. The calcium-based adsorbent enters the conditioning reaction tower and undergoes acidification reaction with the acetic acid wastewater. After conditioning, the adsorbent enters the dry distillation reaction tower for carbonization, recovers the acetone released by the conditioning adsorbent, and then undergoes calcination/carbonation reaction cycle capture CO 2 .
采用乙酸废水调质钙基吸附剂具体的操作方法如下所述：在常温常压条件下，将乙酸废水溶液置于容器内，将石灰石、白云石及氧化钙等钙基吸附剂颗粒加入乙酸废水中，边加入边搅拌，乙酸废水中乙酸与钙基吸附剂中Ca的摩尔比高于1.5∶1，在反应过程中搅拌使钙基吸附剂与乙酸废水反应均匀，反应5小时后，将容器内的反应产物进行加热干燥脱水。乙酸废水调质钙基吸附剂后得到的反应产物在380℃左右能释放出丙酮，采用干馏的方法可回收丙酮，剩余固体产物作为CO2吸附剂。The specific operation method of using acetic acid wastewater to condition the calcium-based adsorbent is as follows: under normal temperature and pressure conditions, the acetic acid wastewater solution is placed in a container, and calcium-based adsorbent particles such as limestone, dolomite and calcium oxide are added to the acetic acid wastewater During the reaction, stir while adding, the molar ratio of acetic acid in the acetic acid wastewater to Ca in the calcium-based adsorbent is higher than 1.5:1, stir during the reaction to make the calcium-based adsorbent and the acetic acid wastewater react evenly, after 5 hours of reaction, the container The reaction product inside is heated and dried for dehydration. The reaction product obtained after conditioning calcium-based adsorbent by acetic acid wastewater can release acetone at about 380°C, acetone can be recovered by dry distillation, and the remaining solid product is used as CO2 adsorbent.
在循环煅烧/碳酸化反应过程中，对采用乙酸溶液调质后的石灰石和原石灰石的循环碳酸化转化率进行实验测定，如表1所示；对采用乙酸溶液调质后的白云石和原白云石的循环碳酸化转化率进行实验测定，结果见表2。实验条件为：煅烧温度为920℃，煅烧气氛为80％CO2和20％O2，碳酸化温度为650～700℃，碳酸化气氛为15％CO2和85％N2。不难发现，经乙酸溶液调质后钙基吸附剂在循环煅烧/碳酸化过程中的碳酸化转化率得到了明显的提高。In the cyclic calcination/carbonation reaction process, the cyclic carbonation conversion rate of limestone and original limestone after acetic acid solution conditioning is experimentally determined, as shown in table 1; The cycle carbonation conversion rate of rock was measured experimentally, and the results are shown in Table 2. The experimental conditions are as follows: the calcination temperature is 920°C, the calcination atmosphere is 80% CO 2 and 20% O 2 , the carbonation temperature is 650-700°C, and the carbonation atmosphere is 15% CO 2 and 85% N 2 . It is not difficult to find that the carbonation conversion rate of calcium-based adsorbents in the cyclic calcination/carbonation process has been significantly improved after conditioning with acetic acid solution.
表1乙酸溶液调质后的石灰石和原石灰石的碳酸化转化率The carbonation conversion rate of limestone and original limestone after the conditioning of table 1 acetic acid solution
表2乙酸溶液调质后的白云石和原白云石的碳酸化转化率Carbonation conversion rate of dolomite and original dolomite after conditioning and tempering by acetic acid solution in table 2
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