CN105727686A - 一种吸附提纯六氟化硫的方法 - Google Patents
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- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/45—Compounds containing sulfur and halogen, with or without oxygen
- C01B17/4507—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only
- C01B17/4515—Compounds containing sulfur and halogen, with or without oxygen containing sulfur and halogen only containing sulfur and fluorine only
- C01B17/453—Sulfur hexafluoride
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Abstract
本发明提供了一种吸附提纯六氟化硫的方法：在反应釜中，加入水滑石，羟丙基?β?环糊精，升温至反应温度，反应结束后静置，再加入1?丁基?3?甲基咪唑的氢氧化物，乙醇，升温至反应温度，待反应结束，再加入四甲基胍乳酸盐，1?胺丙基?3?甲基咪唑四氟硼酸盐，升温至反应温度反应，产物经分离、烘干得到所述吸附剂；工业级六氟化硫经过装有吸附剂的层析柱中进行吸附，吸附后的吸附剂使用氮气脱吸，再除去氮气后得到高纯六氟化硫产品。
Description
技术领域
本发明涉及一种提纯的方法，特别是一种吸附提纯六氟化硫的方法。
背景技术
随着电力系统高压、大容量电网的不断发展，变电站无油化改造进程的加快，高绝缘性能和灭弧性能的气体组合电器应运而生，而六氟化硫(SF6)气体是现阶段能够合成并得到广泛应用的最佳气体灭弧介质。纯净的六氟化硫气体是一种无色无味化学性质非常稳定的物质，它能抵抗熔融的KOH或者500℃水蒸气的作用，它和氧的反应只有在通电、铂丝引爆的情况下才能进行。其主要用于大型发电厂的介电绝缘介质，在半导体制造业中也面临强劲的需求。六氟化硫还可以用作大气扩散试验示踪剂，冶炼镁、铝及其合金的防氧剂以及超声微泡造影剂。此外，它在航空航天、机器制造、医学等其他生产、科研部门中的应用也正在扩展中。
CN102765701A公开了一种六氟化硫气体提纯方法和净化提纯固化罐。用压缩机将六氟化硫吸入六氟化硫分解产物过滤气室，利用专用的吸附剂将六氟化硫中的水分、分解产物及有毒物质进行吸附处理，然后对六氟化硫气体进行加压、制冷，使其液化，液态六氟化硫进入固化罐，使用液氮对六氟化硫进行进一步冷却，温度低于六氟化硫的凝固点后六氟化硫变为固体，此时空气和二氧化碳等杂质气体仍为气体，利用抽真空装置将杂质气体抽出。开启加热装置固体融化后即可得到高纯度的六氟化硫液体，利用专用压缩机构将液态六氟化硫从出液口抽出，进行回充或灌装至钢瓶中。本发明具有处理效率高，处理后气体纯度高，尾气无污染等优点。
CN101857202A公开了一种六氟化硫的提纯方法及其设备，将粗品六氟化硫引入预冷器(1)，将部分或全部六氟化硫液化；液化后的粗品六氟化硫依次通过第一除轻精馏塔(21)、第一除重精馏塔(3)、第二除轻精馏塔(4)，最后经低温换热器(5)换热后灌装。第一除轻精馏塔(2)、第二除轻灌馏塔(4)塔顶的低沸点富集气经尾气捕集器(6)收集处理后，可返回第一除轻精馏塔(2)再利用；第一除轻精馏塔(2)塔釜部分高沸点富集气和第一除重精馏塔(3)塔釜全部高沸点富集气经第二除重精馏塔(7)收集处理后，可返回第一除重精馏塔。大大降低了六氟化硫与能量的损耗。
现有技术中的六氟化硫气体提纯方法，主要利用精馏方法，能耗较大；或者使用碱金属或者碱土金属的氢氧化物、氧化物、活性铝、沸石等吸附，吸附效果难以达到六氟化硫气体体积含量99.99％以上的水平。
发明内容
本发明目的在于解决现有技术中存在的上述技术问题，提供一种吸附提纯六氟化硫的方法。
本发明所述的一种吸附提纯六氟化硫的方法，通过以下步骤制备：
步骤1.负载操作：
将水滑石，占水滑石质量0.5-2％的羟丙基-β-环糊精，50-80℃反应10-24h，静置20-60h；再加入占水滑石质量5-15％的1-丁基-3-甲基咪唑的氢氧化物，占水滑石质量200-500％乙醇，40-80℃反应5-20h，然后加入占水滑石质量0.5-2％的四甲基胍乳酸盐，占水滑石质量0.5％-2％的1-胺丙基-3-甲基咪唑四氟硼酸盐，40-80℃反应10-20h，产物经分离、烘干，得到所述的吸附剂；
步骤2.吸附提纯六氟化硫：
在100～200℃，0.2-1MPa条件下，工业级六氟化硫经过装有吸附剂的层析柱中进行吸附，流速1-5BV/h，吸附后的吸附剂使用氮气脱吸，再除去氮气后得到产品。
本发明中所使用的1-丁基-3-甲基咪唑的氢氧化物，四甲基胍乳酸盐，1-胺丙基-3-甲基咪唑四氟硼酸盐为市售产品，如中科院兰州化学物理研究所的产品；所述水滑石为市售产品，如靖江市康高特塑料科技有限公司的产品；羟丙基-β-环糊精为市售产品，如西安得力生物化工有限公司。
所述工业级六氟化硫为市售产品。
与现有技术相比，本发明的催化剂及其制备方法，具有以下有益效果：
水滑石经过羟丙基-β-环糊精插层改性后，负载引入咪唑基团，可提高吸附气体杂质的能力，六氟化硫气体体积含量大于99.99％。
具体实施方式
以下实例仅仅是进一步说明本发明，并不是限制本发明保护的范围。
实施例1：
步骤1.负载操作：
在1000L反应釜中，将100Kg水滑石，1Kg羟丙基-β-环糊精在60℃条件下反应15h，静止40h，再加入10Kg 1-丁基-3-甲基咪唑的氢氧化物，300Kg乙醇，在60℃条件下反应15h，再加入1Kg四甲基胍乳酸盐，1Kg 1-胺丙基-3-甲基咪唑四氟硼酸盐，在60℃条件下反应15h，分离产物，烘干，得到所述吸附剂。
步骤2.吸附提纯六氟化硫：
在150℃，0.5MPa条件下，工业级六氟化硫经过装有100Kg吸附剂的500L层析柱中进行吸附，流速4BV/h，吸附后的吸附剂使用氮气脱吸，除去氮气后气体经过气相色谱检测，六氟化硫纯度见表1，编号为M-1。
实施例2：
步骤1.负载操作：
在1000L反应釜中，将100Kg水滑石，0.5Kg羟丙基-β-环糊精在50℃条件下反应10h，静止20h，再加入5Kg 1-丁基-3-甲基咪唑的氢氧化物，200Kg乙醇，在40℃条件下反应5h，再加入0.5Kg四甲基胍乳酸盐，0.5Kg 1-胺丙基-3-甲基咪唑四氟硼酸盐，在40℃条件下反应10h，分离产物，烘干，得到所述吸附剂。
步骤2.吸附提纯三氟化氮：
在100℃，0.2MPa条件下，工业级六氟化硫经过装有100Kg吸附剂的500L层析柱中进行吸附，流速1BV/h，吸附后的吸附剂使用氮气脱吸，除去氮气后气体经过气相色谱检测，六氟化硫纯度见表1，编号为M-2。
实施例3
步骤1.负载操作：
在1000L反应釜中，将100Kg水滑石，2Kg羟丙基-β-环糊精在80℃条件下反应24h，静止60h，再加入15Kg 1-丁基-3-甲基咪唑的氢氧化物，500Kg乙醇，在80℃条件下反应20h，再加入0.5Kg四甲基胍乳酸盐，2Kg 1-胺丙基-3-甲基咪唑四氟硼酸盐，在80℃条件下反应10h，分离产物，烘干，得到所述吸附剂。
步骤2.吸附提纯三氟化氮：
在200℃，1MPa条件下，工业级六氟化硫经过装有100Kg吸附剂的500L层析柱中进行吸附，流速5BV/h，吸附后的吸附剂使用氮气脱吸，除去氮气后气体经过气相色谱检测，六氟化硫纯度见表1，编号为M-3。
对比例1
不加入羟丙基-β-环糊精，其它同实施例1。六氟化硫纯度见表1，编号为M-4。
对比例2
不加入1-丁基-3-甲基咪唑的氢氧化物，其它同实施例1。六氟化硫纯度见表1，编号为M-5。
对比例3
不加入四甲基胍乳酸盐，其它同实施例1。六氟化硫纯度见表1，编号为M-6。
对比例4
不加入1-胺丙基-3-甲基咪唑四氟硼酸盐，其它同实施例1。六氟化硫纯度见表1，编号为M-7。
经过气相色谱检测，实施例1-3以及对比例1-3吸附后六氟化硫气体纯度的比较见表1：
表1：不同工艺做出的试验样品吸附后六氟化硫气体纯度的比较
| 编号 | 六氟化硫气体纯度％ |
| M-1 | 99.99 |
| M-2 | 99.97 |
| M-3 | 99.99 |
| M-4 | 98.08 |
| M-5 | 96.81 |
| M-6 | 97.98 |
| M-7 | 98.16 |
以上仅为本发明的具体实施例，但本发明的技术特征并不局限于此。任何以本发明为基础，为解决基本相同的技术问题，实现基本相同的技术效果，所作出的简单变化、等同替换或者修饰等，皆涵盖于本发明的保护范围之中。
Claims (1)
1.一种吸附提纯六氟化硫的方法，其特征在于包括以下步骤：
步骤1.负载操作：
将水滑石，占水滑石质量0.5-2％的羟丙基-β-环糊精，50-80℃反应10-24h，静止20-60h；再加入占水滑石质量5-15％的1-丁基-53-甲基咪唑的氢氧化物，占水滑石质量200-500％乙醇，40-80℃反应5-20h，然后加入占水滑石质量0.5-2％的四甲基胍乳酸盐，占水滑石质量0.5％-2％的1-胺丙基-3-甲基咪唑四氟硼酸盐，40-80℃反应10-20h，产物经分离、烘干，得到所述的吸附剂；
步骤2.吸附提纯六氟化硫：
在100～200℃，0.2-1MPa条件下，工业级六氟化硫经过装有吸附剂的层析柱中进行吸附，流速1-5BV/h，吸附后的吸附剂使用氮气脱吸，再除去氮气后得到产品。
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