甲烷水合物生成的静态强化技术
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摘要
水合物技术可以应用在天然气储运、二氧化碳捕获与封存、海水淡化、混合气分离以及蓄冷等领域。然而，水合物生成时缓慢的传质与传热过程已经成为水合物技术应用的一大障碍。传统的机械扰动、添加简单结构导热填料的方法能够较好的在传质或传热上促进气体水合物生成，但机械扰动要引入更多的能耗和设备，简单导热填料的换热效率低。鉴于此，本文从强化传质与传热两方面探索利于水合物高效生成的静态体系，以甲烷为存储对象，研究甲烷水合物在静态体系中的生成特性。
向纯水中引入疏水性纳米二氧化硅，并高速搅拌分散成具有高比表面积的“硅包水”型水微滴——干水。分散性能优异的干水能够增强水合体系的气-液接触，降低水合诱导时间，促进甲烷水合物快速生成，并提高储气量。但干水经低温水合-升温分解后，其自身“硅包水”的微滴结构被破坏，水从二氧化硅的包囊中溢出、聚集，并形成连续的液态水，使干水的分散性变得很差，基本丧失再次储气的功能，不具有可逆储气的前景。
向纯水中加入结冷胶形成胶冻，再与疏水性纳米二氧化硅在搅拌器中混合分散，制备成一种有支撑结构的改性干水微滴——凝胶干水。凝胶干水继承了干水良好的分散性，能够强化水合体系的气-液接触，加速水合反应，并保持较高的储气量，而且被凝胶支撑的水微滴经水合-分解后的粘连程度比干水低，储气结束后能够保持一定的分散性，可以比较稳定的储气4~6次，但其储气量和储气速率存在一定的衰减。与干水储气性能相比，凝胶干水的一次储气量和最大储气速率都低，主要是由于被结冷胶支撑固定的部分水不易参与水合反应所致。
向浓度0.03wt%的十二烷基硫酸钠（SDS）溶液中引入不同质量比例的疏水性纳米二氧化硅，在搅拌器中分散成另一种改性干水微滴——SDS干溶液。SDS干溶液不仅具有干水的高度分散性，而且每个微滴又具有SDS溶液的表面活性，该体系能够从宏观和微观两方面促进水合体系的气-液接触，提高甲烷水合速率和储气量。不同硅含量的SDS干溶液分散效果不同，但各自的储气速率与同浓度的SDS溶液的水合储气速率相当，比同浓度的SDS溶液储气量高。硅含量7.5wt%的SDS干溶液分散效果好、含水量高，对甲烷的储存量最高，与相同硅含量的干水储气量相当，但比干水储气速率高约1倍。因此，SDS干溶液在促进水合物储气过程中，结合了干水与表面活性剂溶液各自的储气优势，但其储气后也会出现类似干水结构被破坏的现象。
将多孔泡沫铝浸入到浓度0.03wt%的SDS溶液中，其丰富的金属表面可以将水合过程中的热量快速疏导出去，使含泡沫铝的SDS溶液储气速率比单纯的SDS溶液储气速率更大。泡沫铝对SDS溶液水合储气速率的提高率随操作压力的增加而降低，而且对于水合压力推动力过小而不易水合储气的SDS溶液，泡沫铝的加入还有促进水合物成核的作用，主要归功于其粗糙的金属表面能够提供水合结晶点。用填充相为球形的两相复合模型计算甲烷水合物-泡沫铝“复合材料”的导热系数后发现，其有效导热系数是纯甲烷水合物导热系数的132倍。
将干水和凝胶干水分别填充到高孔隙率的泡沫铜中，导热性优异的泡沫铜金属骨架可以将两个水合体系中的水合热及时疏导出去，使含泡沫铜的干水或凝胶干水体系比各自不含泡沫铜的体系储气速率高。泡沫铜对两个分散体系最大水合速率的提高率随着压力的增加而变大。虽然泡沫铜有稳定的金属网络骨架，但对干水或凝胶干水体系均没有支撑作用，两个体系的水微滴也分别会出现类似于干水和凝胶干水储气后粘结、聚集的现象，而且这种现象比单独的干水或凝胶干水体系更严重，使两个体系的再次储气性更差。
以上几个静态水合体系通过强化气-液接触（传质）或强化水合热快速导出（传热）或二者同时强化，促进了甲烷水合物生成，提高了水合储甲烷量，对水合物的大规模生产具有重要的指导意义。
Gas hydrates technology can be contributed to many fields, such as natural gas storage andtransportation, carbon dioxide capture and sequestration, seawater desalination, mixture gasseparation and cold storage in the form of hydrate. However, hydrate formation has beencritically challenged by its poor rate of mass and heat transfer. Mechanical methods andsimple-structure metal fills are often employed in experimental operations to enchancehydrate formation. However, the substantial cost of mechanical devices and energyrequirements may be an unwise payment in real gas storage application. The efficiency ofenhancing heat transfer by simple-strcuture metal fills is also very poor. Hence, in this paer,properties of methane storage in the form of hydrate in static systems were conducted tostudy.
Dry water (DW) with high specific surface was prepared by mixing water, hydrophobicSiO2nanoparticles and air at high speeds. Hydrophobic SiO2particles can encapsulateisolated macroscopic water droplets. Dispersed DW can dramatically reduce the inductiontime and enhance the formation rate of methane hydrare by increasing gas-liquid contactsunder static conditions. However, the capsule-structure water droplets were destabilized byhydration-dissociation process. Most of destroyed DW droplets were connected together andformed continuous liquid phase. The rest DW droplets and continuous water has poorperproties of gas storage and little prospect of reversible storage.
Gel-supporting dry water (GDW) with high specific surface was fomed by mixing water,SiO2nanoparticles, Gellan gun powder and air at high speeds. The modified dry water aremicro-hygrophanous gel particles encapsulated by hydrophobic SiO2particles and also owngood dispersion. GDW can accelerate methane hydrate formation by enhancing contacts ofmethane and hygrophanous gel particles. After hydrate dissociation, some GDW particlesalso connected together and became agglomerative gel particles; the others still kept gooddispersion and can store methane for4~6times due to the supporting action of gel. ThoughGDW primarily realized reversible methane storage, the storage capacity/rate was inferior tothat of DW and decay of storage capacity/rate existed in GDW system.
Another modified dry water, dry solution (DS), was prepared by mixing0.03wt%sodium dodecyl sulfate (SDS) solution, hydrophobic SiO2nanoparticles and air in a high speedblender. SDS-DS combined the good dipersity of DW and the surface activity of SDSsolution. Each SDS-DS droplet can be considered as a micro system of surfactant solution.SDS-DS can enhance gas-liquid contacts and promote methane hyrate formation formmacroscopic and microscopic aspects. The dispersion effect of SDS-DS samples with variouscontents of SiO2was different, but no obvious kinetic differences of hydrate formation wereobserved among them. Rates of methane hydrate formation in these SDS-DS systems were allnearly equivalent to that of single SDS solution and all storage capacities were higher thanthat of SDS solution. The sample with7.5wt%SiO2exhibited about the same CH4storagecapacity as dry water (7.5wt%SiO2), but about twice faster rate than dry water. ThoughSDS-DS combined the advantages of dispersed liquid and surfactant solution, thecapsule-structure of droplets was still destabilized after hydrate dissociation.
Aluminum foam (AF) can provide numerous natural micro vessels with excellent thermalconductivity wall. The addition of AF into SDS solution can promoted hydration heatremoval and accelerate methane hydrate formatioin. The acceleration effect of SDS-AF onhydrate formation is superior to that of SDS itself. Increment fractions of maximum hydrationrates in the presence of AF became smaller with the increasing pressure. Under low pressure,the addition of AF also can promote hydrate nucleation due to its rough metal surface. Areliable heat conduction model based on two-phase materials with spherical inclusions hasbeen applied to determine the effective thermal conductivity (ETC) of hydrate-AF―composites‖. The predicted ETC of composites was132times higher than the thermalconductivity of methane hydrate.
The systems of copper foam (CF) filled with DW or GDW exhibited better storage ratecompared to single DW systems or GDW systems, respectively, because the addition of CFaccelerated hydration heat transfer. For each system, the increment fraction of maximumhydration rates in the presence of CF became greater with the increasing pressure. The metalframework of CF can not play a supporting action in DW or GDW systems and thecapsule-strcuture of droplets in the two systems was also destroyed after hydrate dissociation.The destruction degree was more serious than the systems without CF.
Fast methane storage was achieved in above static systems by enhancing gas-liquid contacts and removing the hydration heat timely, which can provide significance informationon large-scale production of hydrate.
向纯水中引入疏水性纳米二氧化硅，并高速搅拌分散成具有高比表面积的“硅包水”型水微滴——干水。分散性能优异的干水能够增强水合体系的气-液接触，降低水合诱导时间，促进甲烷水合物快速生成，并提高储气量。但干水经低温水合-升温分解后，其自身“硅包水”的微滴结构被破坏，水从二氧化硅的包囊中溢出、聚集，并形成连续的液态水，使干水的分散性变得很差，基本丧失再次储气的功能，不具有可逆储气的前景。
向纯水中加入结冷胶形成胶冻，再与疏水性纳米二氧化硅在搅拌器中混合分散，制备成一种有支撑结构的改性干水微滴——凝胶干水。凝胶干水继承了干水良好的分散性，能够强化水合体系的气-液接触，加速水合反应，并保持较高的储气量，而且被凝胶支撑的水微滴经水合-分解后的粘连程度比干水低，储气结束后能够保持一定的分散性，可以比较稳定的储气4~6次，但其储气量和储气速率存在一定的衰减。与干水储气性能相比，凝胶干水的一次储气量和最大储气速率都低，主要是由于被结冷胶支撑固定的部分水不易参与水合反应所致。
向浓度0.03wt%的十二烷基硫酸钠（SDS）溶液中引入不同质量比例的疏水性纳米二氧化硅，在搅拌器中分散成另一种改性干水微滴——SDS干溶液。SDS干溶液不仅具有干水的高度分散性，而且每个微滴又具有SDS溶液的表面活性，该体系能够从宏观和微观两方面促进水合体系的气-液接触，提高甲烷水合速率和储气量。不同硅含量的SDS干溶液分散效果不同，但各自的储气速率与同浓度的SDS溶液的水合储气速率相当，比同浓度的SDS溶液储气量高。硅含量7.5wt%的SDS干溶液分散效果好、含水量高，对甲烷的储存量最高，与相同硅含量的干水储气量相当，但比干水储气速率高约1倍。因此，SDS干溶液在促进水合物储气过程中，结合了干水与表面活性剂溶液各自的储气优势，但其储气后也会出现类似干水结构被破坏的现象。
将多孔泡沫铝浸入到浓度0.03wt%的SDS溶液中，其丰富的金属表面可以将水合过程中的热量快速疏导出去，使含泡沫铝的SDS溶液储气速率比单纯的SDS溶液储气速率更大。泡沫铝对SDS溶液水合储气速率的提高率随操作压力的增加而降低，而且对于水合压力推动力过小而不易水合储气的SDS溶液，泡沫铝的加入还有促进水合物成核的作用，主要归功于其粗糙的金属表面能够提供水合结晶点。用填充相为球形的两相复合模型计算甲烷水合物-泡沫铝“复合材料”的导热系数后发现，其有效导热系数是纯甲烷水合物导热系数的132倍。
将干水和凝胶干水分别填充到高孔隙率的泡沫铜中，导热性优异的泡沫铜金属骨架可以将两个水合体系中的水合热及时疏导出去，使含泡沫铜的干水或凝胶干水体系比各自不含泡沫铜的体系储气速率高。泡沫铜对两个分散体系最大水合速率的提高率随着压力的增加而变大。虽然泡沫铜有稳定的金属网络骨架，但对干水或凝胶干水体系均没有支撑作用，两个体系的水微滴也分别会出现类似于干水和凝胶干水储气后粘结、聚集的现象，而且这种现象比单独的干水或凝胶干水体系更严重，使两个体系的再次储气性更差。
以上几个静态水合体系通过强化气-液接触（传质）或强化水合热快速导出（传热）或二者同时强化，促进了甲烷水合物生成，提高了水合储甲烷量，对水合物的大规模生产具有重要的指导意义。
Gas hydrates technology can be contributed to many fields, such as natural gas storage andtransportation, carbon dioxide capture and sequestration, seawater desalination, mixture gasseparation and cold storage in the form of hydrate. However, hydrate formation has beencritically challenged by its poor rate of mass and heat transfer. Mechanical methods andsimple-structure metal fills are often employed in experimental operations to enchancehydrate formation. However, the substantial cost of mechanical devices and energyrequirements may be an unwise payment in real gas storage application. The efficiency ofenhancing heat transfer by simple-strcuture metal fills is also very poor. Hence, in this paer,properties of methane storage in the form of hydrate in static systems were conducted tostudy.
Dry water (DW) with high specific surface was prepared by mixing water, hydrophobicSiO2nanoparticles and air at high speeds. Hydrophobic SiO2particles can encapsulateisolated macroscopic water droplets. Dispersed DW can dramatically reduce the inductiontime and enhance the formation rate of methane hydrare by increasing gas-liquid contactsunder static conditions. However, the capsule-structure water droplets were destabilized byhydration-dissociation process. Most of destroyed DW droplets were connected together andformed continuous liquid phase. The rest DW droplets and continuous water has poorperproties of gas storage and little prospect of reversible storage.
Gel-supporting dry water (GDW) with high specific surface was fomed by mixing water,SiO2nanoparticles, Gellan gun powder and air at high speeds. The modified dry water aremicro-hygrophanous gel particles encapsulated by hydrophobic SiO2particles and also owngood dispersion. GDW can accelerate methane hydrate formation by enhancing contacts ofmethane and hygrophanous gel particles. After hydrate dissociation, some GDW particlesalso connected together and became agglomerative gel particles; the others still kept gooddispersion and can store methane for4~6times due to the supporting action of gel. ThoughGDW primarily realized reversible methane storage, the storage capacity/rate was inferior tothat of DW and decay of storage capacity/rate existed in GDW system.
Another modified dry water, dry solution (DS), was prepared by mixing0.03wt%sodium dodecyl sulfate (SDS) solution, hydrophobic SiO2nanoparticles and air in a high speedblender. SDS-DS combined the good dipersity of DW and the surface activity of SDSsolution. Each SDS-DS droplet can be considered as a micro system of surfactant solution.SDS-DS can enhance gas-liquid contacts and promote methane hyrate formation formmacroscopic and microscopic aspects. The dispersion effect of SDS-DS samples with variouscontents of SiO2was different, but no obvious kinetic differences of hydrate formation wereobserved among them. Rates of methane hydrate formation in these SDS-DS systems were allnearly equivalent to that of single SDS solution and all storage capacities were higher thanthat of SDS solution. The sample with7.5wt%SiO2exhibited about the same CH4storagecapacity as dry water (7.5wt%SiO2), but about twice faster rate than dry water. ThoughSDS-DS combined the advantages of dispersed liquid and surfactant solution, thecapsule-structure of droplets was still destabilized after hydrate dissociation.
Aluminum foam (AF) can provide numerous natural micro vessels with excellent thermalconductivity wall. The addition of AF into SDS solution can promoted hydration heatremoval and accelerate methane hydrate formatioin. The acceleration effect of SDS-AF onhydrate formation is superior to that of SDS itself. Increment fractions of maximum hydrationrates in the presence of AF became smaller with the increasing pressure. Under low pressure,the addition of AF also can promote hydrate nucleation due to its rough metal surface. Areliable heat conduction model based on two-phase materials with spherical inclusions hasbeen applied to determine the effective thermal conductivity (ETC) of hydrate-AF―composites‖. The predicted ETC of composites was132times higher than the thermalconductivity of methane hydrate.
The systems of copper foam (CF) filled with DW or GDW exhibited better storage ratecompared to single DW systems or GDW systems, respectively, because the addition of CFaccelerated hydration heat transfer. For each system, the increment fraction of maximumhydration rates in the presence of CF became greater with the increasing pressure. The metalframework of CF can not play a supporting action in DW or GDW systems and thecapsule-strcuture of droplets in the two systems was also destroyed after hydrate dissociation.The destruction degree was more serious than the systems without CF.
Fast methane storage was achieved in above static systems by enhancing gas-liquid contacts and removing the hydration heat timely, which can provide significance informationon large-scale production of hydrate.
引文
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