CN104437443B - 一种提高吸附材料存储天然气性能的活化方法 - Google Patents
一种提高吸附材料存储天然气性能的活化方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 32
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000003345 natural gas Substances 0.000 title claims abstract description 14
- 230000004913 activation Effects 0.000 title claims abstract description 12
- 238000003860 storage Methods 0.000 title claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 15
- 235000002639 sodium chloride Nutrition 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 238000010306 acid treatment Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 150000003839 salts Chemical class 0.000 claims abstract description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims abstract description 8
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims abstract description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 4
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 4
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 4
- 239000001103 potassium chloride Substances 0.000 claims abstract description 4
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 4
- 239000011780 sodium chloride Substances 0.000 claims abstract description 4
- 239000004317 sodium nitrate Substances 0.000 claims abstract description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229910021536 Zeolite Inorganic materials 0.000 claims description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 5
- 239000010457 zeolite Substances 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000000243 solution Substances 0.000 claims description 3
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 239000003456 ion exchange resin Substances 0.000 claims description 2
- 229920003303 ion-exchange polymer Polymers 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 1
- 239000012266 salt solution Substances 0.000 claims 1
- 239000011734 sodium Substances 0.000 claims 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 claims 1
- 235000011118 potassium hydroxide Nutrition 0.000 abstract description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 abstract description 3
- 235000011121 sodium hydroxide Nutrition 0.000 abstract description 3
- 229910052938 sodium sulfate Inorganic materials 0.000 abstract description 3
- 235000011152 sodium sulphate Nutrition 0.000 abstract description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
- 238000002336 sorption--desorption measurement Methods 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 10
- -1 NACF Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012621 metal-organic framework Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000004965 peroxy acids Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910001868 water Inorganic materials 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
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Abstract
本发明公开了一种提高吸附材料存储天然气性能的活化方法。本方法分为焙烧、酸处理、碱处理、盐处理四道工序，由盐酸、硝酸和氢氟酸配制的浓度为0.5～2.0mol/L酸溶液，和由氢氧化钠、氢氧化钾、氢氧化铵配制的浓度为0.5～2.5 mol/L碱溶液，以及氯化钠、氯化钾、氯化铵、硫酸钠、硫酸铵、硝酸钠、硝酸铵配制的盐溶液，分别对经过300～890℃焙烧后的吸附材料，进行活化处理。依此方法生产可获得具有高比表面积、天然气存储能力高、吸脱附性能良好、使用寿命长的高效天然气吸附材料。
Description
技术领域
本发明涉及吸附材料的活化处理方法，具体涉及为提高天然气吸附材料的活化方法，属于吸附材料技术领域。
背景技术
在吸附式存储天然气的研究中, 最主要的核心工作是高性能吸附剂的开发和其制备工艺的优化、调控，尤其对吸附材料的活化处理方法最为关键。
存储天然气的吸附材料被广泛开发和利用，如天然沸石、分子筛、活性氧化铝、硅胶、炭黑、活性炭、活性炭纤维、金属有机框架化合物等。但是目前被报道的吸附剂，其吸附性能还不是很理想。在吸附材料的活化处理中，活化方法主要为物理法( 水蒸气活化法、二氧化碳活化法和空气活化法等) 和化学法( 磷酸法、氯化锌法、氢氧化钾和碳酸钾等)。在不作任何处理时，吸附材料的孔、通道中往往被钙、镁等阳离子、水和有机物分子以及无机杂质所占据，孔通道被堵塞，活性位减少。因此，寻找合适的活化方法对吸附材料进行处理，以提高吸附材料的吸附性能成为必要。
发明内容
本发明公开一种天然气吸附材料的活化处理方法，其特征在于活化经焙烧、酸处理、碱处理、盐处理四道工序。每个工序为独立实施，并且为后序操作提供基础。在实际生产工艺中，可连续生产亦可间歇生产。
本发明的吸附材料不局限于炭基吸附材料，适应于天然沸石、分子筛、活性氧化铝、活性炭、活性炭纤维、石墨烯、离子交换树脂等吸附材料，尤其对沸石、活性炭吸附材料效果更佳。
本发明方法快速、简便，工艺流程短，同时经过本发明活化处理后的吸附材料，具有如下特点：
(1)具有高的比表面积和发达的微孔结构；
(2)吸附容量大，在3.5MPa下，吸附材料具有100 (体积比)以上的天然气有效存储能力；
(3)吸附和脱附的速率快，当压力下降到常压时，吸附剂内残留的“余气”少；
(4)导热性良好，使用寿命长，且能再生使用；
本发明通过以下方法实现：
首先，对经过预先制备的天然气吸附材料进行高温焙烧，焙烧的目的是清除材料孔穴和孔道的有机物等，焙烧温度为300～890℃，时间为2-8小时；
其次，对焙烧后的天然气吸附材料进行酸处理。酸处理工序所用酸为盐酸、硝酸和氢氟酸的水溶液，所配得到酸溶液浓度为0.5～2.0 mol/L，酸处理时间为2.5-16小时。
经过酸处理以达到如下目的：
(1) 清除天然气吸附材料孔穴和孔道的无机和有机杂质, 从而使孔穴和孔道得到疏通；
(2) 使半径小的H+ 置换半径大的阳离子, 使孔道的有效空间拓宽；
(3) 增加吸附活性中心。
然后，对吸附材料进行碱处理。调配氢氧化钠、氢氧化钾、氢氧化铵的水溶液，配制的碱溶液浓度为0.5～2.5 mol/L，碱处理时间为3.5-16小时。此条件下，调整了吸附材料的微孔孔径和孔道结构，改善了吸附材料的吸附性能。
最后，对吸附材料进行盐处理。采用一定浓度的无机盐，选用氯化钠、氯化钾、氯化铵、硫酸钠、硫酸铵、硝酸钠、硝酸铵配制盐溶液，配得离子浓度分别为：Na+浓度为0.5～3.0 mol/L，K+浓度为1.0～4.0 mol/L，NH4 +浓度为0.2~2.5 mol/L，盐处理时间为3.5-12小时。
具体实施方式
第一，选取20-100目的天然沸石进行焙烧，焙烧温度为790℃，时间为8小时。
第二，对焙烧后的天然气吸附材料进行酸处理。选用盐酸、硝酸和氢氟酸的水溶液，所配得到酸溶液浓度为1.0 mol/L，酸处理时间为5小时。
第三，调配氢氧化钠、氢氧化钾、氢氧化铵的水溶液，配制的碱溶液浓度为2.5 mol/L，碱处理时间为5小时。
第四，选用氯化钠、氯化钾、氯化铵、硫酸钠、硫酸铵、硝酸钠、硝酸铵配制盐溶液，配得离子浓度分别为：Na+浓度为3.0 mol/L，K+浓度为2.0 mol/L，NH4 +浓度为1.5 mol/L，盐处理时间为10小时。
Claims (1)
1.一种提高吸附材料存储天然气性能的活化方法，其特征在于活化经焙烧、酸处理、碱处理、盐处理四道工序，所述焙烧工序中焙烧温度为300～890℃，时间为2-8小时，所述酸处理工序所用酸为盐酸、硝酸和氢氟酸的水溶液，所配得到酸溶液浓度为0.5～2.0mol/L，酸处理时间为2.5-16小时，所述碱处理所用碱为氢氧化钠、氢氧化钾、氢氧化铵的水溶液，所配碱溶液浓度为0.5～2.5mol/L，碱处理时间为3.5-16小时，所述盐处理所用盐为氯化钠、氯化钾、氯化铵、硫酸钠、硫酸铵、硝酸钠、硝酸铵的水溶液，所配盐溶液中Na+浓度为0.5～3.0mol/L，K+浓度为1.0～4.0mol/L，NH4 +浓度为0.2～2.5mol/L，盐处理时间为3.5-12小时，所述吸附材料为沸石、活性氧化铝、活性炭、石墨烯或离子交换树脂。
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