CN101905320B - Copper powder dry water for improving gas storage rate of hydrate and preparation method and application thereof - Google Patents
Copper powder dry water for improving gas storage rate of hydrate and preparation method and application thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract description 57
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title abstract description 48
- 238000003860 storage Methods 0.000 title abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 19
- 230000002209 hydrophobic effect Effects 0.000 abstract description 16
- 229910021485 fumed silica Inorganic materials 0.000 abstract description 12
- 150000004677 hydrates Chemical class 0.000 abstract description 11
- 238000006703 hydration reaction Methods 0.000 abstract description 9
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 abstract description 5
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 29
- 239000002245 particle Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- NMJORVOYSJLJGU-UHFFFAOYSA-N methane clathrate Chemical compound C.C.C.C.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O NMJORVOYSJLJGU-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000012856 weighed raw material Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009775 high-speed stirring Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
本发明公开了一种能提高水合物储气速率的铜粉干水及其制法和应用。本发明由疏水性气相二氧化硅、铜粉和水组成。疏水性气相二氧化硅占铜粉干水的5％～15％wt，铜粉占5％～20％wt，其余为水。将疏水性气相二氧化硅、铜粉和水混合后在10000～30000r/min下搅拌30～120s即制得铜粉干水。本发明所述的铜粉干水制备工艺简单，可应用于水合物储气领域，能够大幅增加气水接触面积，提高水合物储气速率。铜粉干水中纳米铜粉的存在能够增强导热性使水合反应产生的热量及时传导出去，加速水合反应。The invention discloses copper powder dry water capable of increasing the gas storage rate of hydrates, a preparation method and application thereof. The invention consists of hydrophobic fumed silicon dioxide, copper powder and water. The hydrophobic fumed silica accounts for 5%-15%wt of the dry water of the copper powder, the copper powder accounts for 5%-20%wt, and the rest is water. Mix hydrophobic fumed silica, copper powder and water and stir at 10000-30000r/min for 30-120s to prepare copper powder dry water. The copper powder dry water preparation process of the present invention is simple, can be applied to the field of hydrate gas storage, can greatly increase the gas-water contact area, and improve the hydrate gas storage rate. The presence of nano-copper powder in copper powder dry water can enhance the thermal conductivity, so that the heat generated by the hydration reaction can be conducted out in time, and the hydration reaction can be accelerated.
Description
技术领域 technical field
本发明涉及水合物储气技术领域，具体涉及一种能提高水合物储气速率的铜粉干水及其制法和应用。The invention relates to the technical field of hydrate gas storage, in particular to copper powder dry water capable of increasing the gas hydrate storage rate, its preparation method and application.
背景技术 Background technique
气体水合物是水与甲烷、乙烷、二氧化碳及硫化氢等小分子气体形成的非化学计量的笼型化合物。目前已经已经发现的水合物晶体结构有Ⅰ型、Ⅱ型和H型3种。气体水合物的研究大致可以分为3个阶段：第一阶段为(1810～1934年)实验室研究，主要是科学家出于好奇研究水合物的组成以及那些气体可以形成水合物；第二阶段(1934～1993年)为水合物研究快速发展阶段，主要是确定水合物生成的热力学条件和抑制方法；第三阶段(1993年～至今)水合物生成分解动力学的研究取得重大进展，水合物在储气、蓄冷、分离等方面的潜在应用开始得到广泛关注。Gas hydrate is a non-stoichiometric cage compound formed by water and small molecular gases such as methane, ethane, carbon dioxide and hydrogen sulfide. The crystal structures of hydrates that have been discovered so far include Type I, Type II and Type H. The research on gas hydrates can be roughly divided into three stages: the first stage (1810-1934) laboratory research, mainly for scientists to study the composition of hydrates and those gases that can form hydrates out of curiosity; the second stage ( 1934-1993) was the rapid development stage of hydrate research, mainly to determine the thermodynamic conditions and inhibition methods of hydrate formation; the third stage (1993-present) was the research on the kinetics of hydrate formation and decomposition, which made great progress. Potential applications in gas storage, cold storage, and separation have begun to receive widespread attention.
水合物储气是指在一定温度和压力下使气体作为客体分子进入主体分子水形成的水合物笼型晶格中，通过范德华力作用实现气体储存的一种方法。水合物储气具有安全、清洁高效等优点。标准状况下，1体积的甲烷水合物能够储存大约180体积的甲烷。目前利用水合物储气存在的缺点主要有：(1)气水接触面积小，反应速率慢(2)水合物储气量低。为解决气水接触面积小，反应速率慢的问题，科研工作者也采取了一下强化措施，如机械搅拌、喷雾等措施，目前这些措施只能应用于实验室范围，很难工业化。Hydrate gas storage refers to a method in which gas as a guest molecule enters the hydrate cage lattice formed by host molecular water under a certain temperature and pressure, and realizes gas storage through the action of van der Waals force. Hydrate gas storage has the advantages of safety, cleanliness and high efficiency. Under standard conditions, 1 volume of methane hydrate can store about 180 volumes of methane. At present, the main disadvantages of using hydrates for gas storage are: (1) The gas-water contact area is small, and the reaction rate is slow; (2) The gas storage capacity of hydrates is low. In order to solve the problem of small gas-water contact area and slow reaction rate, scientific researchers have also taken some intensive measures, such as mechanical stirring, spraying and other measures. At present, these measures can only be applied in the laboratory and are difficult to industrialize.
干水是水和疏水性气相二氧化硅在空气中高速搅拌形成的一种自由流动的粉末状物质。2009年，王卫星等首次利用干水强化气体水合物的生成，大幅提高了气水接触面积，使反应速率大幅提高，同时也使储气量在短时间内得到提高。Carter等在干水中添加胶凝剂形成干凝胶以提高干水储气的循环利用率。水合反应是一种放热反应，上述研究都没有考虑水合物储气时产生的热效应，若放出的热量不能及时排出，会使水合反应速率降低，影响储气效果。Dry water is a free-flowing powdery substance formed by high-speed stirring of water and hydrophobic fumed silica in air. In 2009, Wang Weixing and others used dry water to enhance the formation of gas hydrate for the first time, which greatly increased the gas-water contact area, greatly increased the reaction rate, and also increased the gas storage capacity in a short period of time. Carter et al. added gelling agent to dry water to form xerogel to improve the recycling rate of dry water gas storage. The hydration reaction is an exothermic reaction. The above studies have not considered the thermal effect of hydrate gas storage. If the released heat cannot be discharged in time, the hydration reaction rate will be reduced and the gas storage effect will be affected.
发明内容 Contents of the invention
本发明一方面在于增大水合物储气时的气水接触面积，另一方面在于将水合反应时产生的热量及时排出，提高水合物反应速率，并且使水合物短时间内的储气量得到提高。On the one hand, the present invention aims to increase the gas-water contact area when hydrate gas is stored, and on the other hand, to discharge the heat generated during hydration reaction in time, improve the reaction rate of hydrate, and increase the gas storage capacity of hydrate in a short time .
本发明利用高强度搅拌器通过高速剪切的方法混合了疏水性纳米级气相二氧化硅粉末、纳米级铜粉和水，制备了一种能提高水合物储气速率的铜粉干水。制备出的铜粉干水颗粒呈固体状态，颗粒尺寸在20～100μm之间，且疏水性纳米级气相二氧化硅颗粒及纳米铜粉分布均匀。The invention mixes hydrophobic nano-scale fumed silicon dioxide powder, nano-scale copper powder and water by a high-intensity stirrer through a high-speed shearing method, and prepares copper powder dry water capable of increasing the gas storage rate of hydrates. The prepared dry water particles of the copper powder are in a solid state, the particle size is between 20 and 100 μm, and the hydrophobic nano-scale fumed silicon dioxide particles and the nano-copper powder are evenly distributed.
本发明所述的的铜粉干水制备工艺简单，可应用于水合物储气领域，能够大幅增加气水接触面积，提高水合物储气速率。铜粉干水中纳米级铜粉的存在能够增强导热性使水合反应产生的热量及时传导出去，加速水合反应。The copper powder dry water preparation process of the present invention is simple, can be applied to the field of hydrate gas storage, can greatly increase the gas-water contact area, and improve the hydrate gas storage rate. The presence of nano-sized copper powder in copper powder dry water can enhance the thermal conductivity, so that the heat generated by the hydration reaction can be conducted in time, and the hydration reaction can be accelerated.
本发明通过以下技术方案来实现：The present invention is realized through the following technical solutions:
一种提高水合物储气速率的铜粉干水，是由疏水性气相二氧化硅、铜粉和水组成。A copper powder dry water for improving the gas storage rate of hydrates is composed of hydrophobic fumed silicon dioxide, copper powder and water.
所述疏水性气相二氧化硅占铜粉干水的5％～15％wt，铜粉占5％～20％wt，其余为水。所述铜粉干水的颗粒尺寸在20～100μm。The hydrophobic fumed silica accounts for 5%-15%wt of the copper powder dry water, the copper powder accounts for 5%-20%wt, and the rest is water. The particle size of the dry water of the copper powder is 20-100 μm.
所述疏水性气相二氧化硅的粒径为7～40nm，比表面积为100～300m2/g。The particle size of the hydrophobic fumed silica is 7-40 nm, and the specific surface area is 100-300 m 2 /g.
所述铜粉的粒径为10～30nm。The particle size of the copper powder is 10-30nm.
所述的铜粉干水的制备方法，包括以下步骤；The preparation method of described copper powder dry water, comprises the following steps;
将疏水性气相二氧化硅、铜粉和水混合后在10000～30000r/min下搅拌30～120s制得铜粉干水。The hydrophobic fumed silica, copper powder and water are mixed and then stirred at 10000-30000r/min for 30-120s to prepare copper powder dry water.
所述疏水性气相二氧化硅占铜粉干水的5％～15％wt，铜粉占5％～20％wt，其余为水。The hydrophobic fumed silica accounts for 5%-15%wt of the copper powder dry water, the copper powder accounts for 5%-20%wt, and the rest is water.
所述疏水性气相二氧化硅的粒径为7～40nm，比表面积为100～300m2/g。The particle size of the hydrophobic fumed silica is 7-40 nm, and the specific surface area is 100-300 m 2 /g.
所述的铜粉干水在水合物储气领中的应用，所述铜粉干水使用温度为-80～30℃，使用压力为0～100MPa。For the application of the copper powder dry water in the hydrate gas storage collar, the use temperature of the copper powder dry water is -80-30° C., and the use pressure is 0-100 MPa.
本发明相对于现有技术具有的优点及有益效果。Compared with the prior art, the present invention has advantages and beneficial effects.
(1)本发明能够大大提高水合物反应时的气水接触面积，提高水合物储气速率和短时间内水合物储气量。铜粉的存在能够增强导热性使水合反应产生的热量及时传导出去，加速水合反应。(1) The present invention can greatly increase the gas-water contact area during the hydrate reaction, increase the gas storage rate of the hydrate and the gas storage capacity of the hydrate in a short time. The presence of copper powder can enhance the thermal conductivity, so that the heat generated by the hydration reaction can be conducted in time, and the hydration reaction can be accelerated.
(2)本发明制备工艺简单，易于大规模生产。(2) The preparation process of the present invention is simple and easy for large-scale production.
具体实施方式 Detailed ways
下面就本发明进一步举例说明，但本发明的实施方式并不仅限于此。The present invention will be further illustrated below, but the embodiments of the present invention are not limited thereto.
实施例1Example 1
(1)用天平分别称取5g粒径范围为7～40nm的疏水性气相二氧化硅粉末、5g粒径范围为10～30nm的纳米级铜粉和90g室温下的去离子水。(1) Weigh 5 g of hydrophobic fumed silica powder with a particle size ranging from 7 to 40 nm, 5 g of nanoscale copper powder with a particle size ranging from 10 to 30 nm, and 90 g of deionized water at room temperature with a balance.
(2)将称取好的原料放入高速搅拌其中，在10000r/min下搅拌30s制得铜粉干水，制得铜粉干水粒径范围为20～100μm。(2) Put the weighed raw materials into high-speed stirring, and stir at 10,000 r/min for 30 seconds to obtain copper powder dry water, and the particle size range of the obtained copper powder dry water is 20-100 μm.
实施例2Example 2
(1)用天平分别称取10g粒径范围为7～40nm的疏水性气相二氧化硅粉末、10g粒径范围为10～30nm的铜粉和80g室温下的去离子水。(1) Use a balance to weigh 10 g of hydrophobic fumed silica powder with a particle size ranging from 7 to 40 nm, 10 g of copper powder with a particle size ranging from 10 to 30 nm, and 80 g of deionized water at room temperature.
(2)将称取好的原料放入高速搅拌其中，在20000r/min下搅拌60s制得铜粉干水，制得铜粉干水粒径范围为20～100μm。(2) Put the weighed raw materials into high-speed stirring, and stir at 20,000 r/min for 60 seconds to obtain copper powder dry water, and the particle size range of the obtained copper powder dry water is 20-100 μm.
实施例3Example 3
(1)用天平分别称取15g粒径范围为7～40nm的疏水性气相二氧化硅粉末、15g粒径范围为10～30nm的铜粉和70g室温下的去离子水。(1) Weigh 15g of hydrophobic fumed silica powder with a particle size range of 7-40nm, 15g of copper powder with a particle size range of 10-30nm and 70g of deionized water at room temperature with a balance.
(2)将称取好的原料放入高速搅拌其中，在25000r/min下搅拌90s制得铜粉干水，制得铜粉干水粒径范围为20～100μm。(2) Put the weighed raw materials into a high-speed stirrer, stir at 25000r/min for 90s to obtain copper powder dry water, and the particle size range of the obtained copper powder dry water is 20-100 μm.
实施例4Example 4
(1)用天平分别称取15g粒径范围为7～40nm的疏水性气相二氧化硅粉末、20g粒径范围为10～30nm的铜粉和65g室温下的去离子水。(1) Weigh 15g of hydrophobic fumed silica powder with a particle size range of 7-40nm, 20g of copper powder with a particle size range of 10-30nm, and 65g of deionized water at room temperature with a balance.
(2)将称取好的原料放入高速搅拌其中，在30000r/min下搅拌120s制得铜粉干水，制得铜粉干水粒径范围为20～100μm。(2) Put the weighed raw materials into a high-speed stirrer, stir at 30000r/min for 120s to obtain copper powder dry water, and the particle size range of the obtained copper powder dry water is 20-100 μm.
实施例1～4制备铜粉干水具体实例见表1：Embodiment 1～4 prepares copper powder dry water concrete example and sees Table 1:
表1 Table 1
将制备好的铜粉干水放入高压水合物反应釜中，用真空泵将反应釜抽真空，然后通入气体甲烷。设定初始温度和压力，然后降温使其生成水合物，待温度和压力稳定，反应结束。The prepared copper powder dry water is put into a high-pressure hydrate reactor, the reactor is evacuated by a vacuum pump, and then gas methane is introduced. Set the initial temperature and pressure, then lower the temperature to form hydrates, and the reaction ends when the temperature and pressure are stable.
制备的铜粉干水储气性能见表2：The dry water gas storage performance of the prepared copper powder is shown in Table 2:
实验结果可以看出，在初始压力为6MPa，反应温度为273.15K条件下，？g铜粉干水能够与甲烷快速反应生成水合物，在反应1.5小时后所有样品的储气量都能够达到最大储气量的80％。其中，样品2的效果最好，反应1.5小时后能达到最大储气量的90％。From the experimental results, it can be seen that under the condition of initial pressure of 6MPa and reaction temperature of 273.15K, ? The dry water of g copper powder can quickly react with methane to form hydrates, and the gas storage capacity of all samples can reach 80% of the maximum gas storage capacity after 1.5 hours of reaction. Among them, sample 2 has the best effect, and can reach 90% of the maximum gas storage capacity after 1.5 hours of reaction.
表2 Table 2
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