CN109529795A - 一种硫化氢吸附剂及其制备方法 - Google Patents
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 56
- 229910000037 hydrogen sulfide Inorganic materials 0.000 title claims abstract description 56
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910001051 Magnalium Inorganic materials 0.000 claims abstract description 20
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 19
- 229960001545 hydrotalcite Drugs 0.000 claims abstract description 19
- 229910001701 hydrotalcite Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 26
- 239000003513 alkali Substances 0.000 claims description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000004530 micro-emulsion Substances 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 9
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 8
- 159000000013 aluminium salts Chemical class 0.000 claims description 7
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 159000000003 magnesium salts Chemical class 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical compound [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 238000001354 calcination Methods 0.000 claims description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 4
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 239000000908 ammonium hydroxide Substances 0.000 claims description 3
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 22
- 239000007789 gas Substances 0.000 abstract description 12
- 239000006185 dispersion Substances 0.000 abstract description 3
- 229910021645 metal ion Inorganic materials 0.000 abstract description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 abstract description 2
- -1 anion forms compound Chemical class 0.000 abstract description 2
- 239000002440 industrial waste Substances 0.000 abstract description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 2
- 239000002594 sorbent Substances 0.000 abstract description 2
- 239000002912 waste gas Substances 0.000 abstract description 2
- 150000004706 metal oxides Chemical class 0.000 abstract 1
- 238000000034 method Methods 0.000 description 13
- 238000006477 desulfuration reaction Methods 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 230000023556 desulfurization Effects 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 239000002250 absorbent Substances 0.000 description 6
- 230000002745 absorbent Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
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- 150000001450 anions Chemical group 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000001172 regenerating effect Effects 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
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- 230000008929 regeneration Effects 0.000 description 4
- 238000011069 regeneration method Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 3
- 239000008246 gaseous mixture Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000001376 precipitating effect Effects 0.000 description 3
- 238000009938 salting Methods 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 231100000572 poisoning Toxicity 0.000 description 2
- 230000000607 poisoning effect Effects 0.000 description 2
- 239000011833 salt mixture Substances 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- ZGBSOTLWHZQNLH-UHFFFAOYSA-N [Mg].S(O)(O)(=O)=O Chemical compound [Mg].S(O)(O)(=O)=O ZGBSOTLWHZQNLH-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 125000001741 organic sulfur group Chemical group 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—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
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28011—Other properties, e.g. density, crush strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
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- B01D2253/1124—Metal oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本发明公开了一种硫化氢吸附剂及其制备方法,属于废气治理技术领域。本发明硫化氢吸附剂化学式为Mg1‑xAlxOm,其中0.2≤x≤0.34,2≤m≤6;本发明的硫化氢吸附剂通过焙烧镁铝二元水滑石前驱体制备而得。本发明镁铝水滑石焙烧脱去层间水、阴离子形成复合铝镁金属氧化物吸附剂,具有比表面积大、热稳定性高、抗烧结能力好的特点,铝镁金属离子可以达到分子和原子级的分散,可作为吸附处理工业废气硫化氢气体的吸附剂。
Description
技术领域
本发明涉及一种硫化氢吸附剂及其制备方法,属于废气治理技术领域。
背景技术
随着石油化工工业的飞速发展,人民生活水平的不断提高,天然气、焦炉气、煤气越来越多的用作石油化工的原料、民用和工业撰料。这些气体中都含有一定数量的硫化氢和有机硫。硫化氢是自然界中一种丰富的潜在资源,具有强烈的臭鸡蛋气味,在湿热条件下会腐蚀设备和管道,缩短设备使用寿命,甚至有可能造成重大事故,是大气污染物中毒性很大的污染之一。原料气中的硫化物能使化学反应的催化剂中毒、腐蚀设备管道、影响产品质量H2S及其燃烧产物SO2是导致大气污染,形成酸雨的主要主要污染源,这些工业装置弛放气排入大气严重地危害人体健康、污染环境。因此,都需要脱除硫化物。其中,最主要的是硫化氢。
目前,脱除H2S的方法很多,按脱硫效果,可分为粗脱、半精脱和精脱;按工艺可分为:再生溶剂吸收脱硫、固定床吸附脱硫、膜分离方法脱硫、生物脱硫、以及物理场脱硫等;根据脱除方法的特点可分为吸收法、吸附法、氧化法、生物法、脉冲电晕法等;依据物质所处的状态又可分为湿法和干法两大类。干法脱硫常用于低含硫气体处理。目前,国内外常用的干法脱硫剂有高温干法脱硫剂和常温干法脱硫剂。对于高温脱硫剂国内开发较少,其中最主要的问题是:能耗大和脱硫剂粉化、再生问题。
常用的脱除H2S的吸附剂有氧化锌、氧化铁、活性炭、分子筛等大颗粒吸附剂,其各有利弊。氧化锌脱硫剂以其脱硫精度高、使用简便、性能稳定可靠、硫容高而占据着重要地位, ZnO吸附剂的主要缺点是不能通过氧化就地再生,须更换新的吸附剂;因为再生中吸附剂表面会因烧结而明显减少,机械强度也大大降低。氧化铁脱硫剂是一种传统的气体净化材料,由于其资源丰富、价格低廉而得到广泛应用,在常温下有良好的脱硫功能,然而在高温下吸附效率低,且吸附后的产物不易再生,不可循环使用。活性炭材料是由石墨微晶和无定形炭构成的一种黑色多孔固体,孔隙结构发达,具有巨大的比表面积,对气体、溶液中的无机或有机物质及胶体颗粒等都有很强的吸附能力,活性炭吸附处理工艺存在的问题是活性炭遇水受潮后容易板结,比表面积大大减少,从而影响到处理效果。当然,活性炭表面吸附过多的污染物之后,其效能也会降低,到一定程度时就必须更换、再生。
发明内容
针对现有技术中硫化氢吸附剂的问题,本发明提供一种硫化氢吸附剂及其制备方法,本发明硫化氢吸附剂利用镁铝水滑石为前躯体制备的镁铝复合氧化物脱硫吸附剂,镁铝水滑石为阴离子型层状化合物,层间具有可交换的阴离子,具有弱碱性;镁铝水滑石具有类似于水镁石[Mg(OH)2]的正八面体结构,镁铝水滑石焙烧脱去层间水、阴离子形成复合铝镁金属氧化物吸附剂,具有比表面积大、热稳定性高、抗烧结能力好的特点,铝镁金属离子可以达到分子和原子级的分散,可作为吸附处理工业废气硫化氢气体的吸附剂。
一种硫化氢吸附剂,化学式为Mg1-xAlxOm,其中0.2≤x≤0.34,2≤m≤6。
所述硫化氢吸附剂的制备方法,具体步骤如下:
(1)将镁盐和铝盐溶解于去离子水中得到混合盐溶液A;其中镁盐为硝酸镁、硫酸镁或氯化镁,铝盐为硝酸铝、硫酸铝或氯化铝;
(2)配制混合碱溶液B,其中混合碱溶液B为氨水、碳酸氢钠、氢氧化钠、碳酸钠的两种以上混合碱溶液;
(3)在搅拌条件下,将步骤(2)的混合碱溶液B与步骤(1)的混合盐溶液A分别逐滴滴入去离子水中使体系的pH值在9~11得到微乳液C;
(4)将步骤(3)的微乳液C置于温度为60~80℃条件下陈化反应16~18h,固液分离,固体水洗至中性,干燥、粉碎即得镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·mH2O;其中x为Al3+的物质量与(Mg2++Al3+)的总物质量的比值,0.2≤x≤0.34;m为结晶水数量,2 ≤m≤6;
(5)将步骤(4)镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·mH2O匀速升温至温度为450℃~650℃并恒温焙烧4~8h,研磨、筛分即得硫化氢吸附剂Mg1-xAlxOm。
所述步骤(1)混合盐溶液A中Al3+的摩尔量与Mg2++Al3+的总摩尔量的比为(0.2~0.34):1。
所述步骤(2)混合碱溶液B中OH-离子摩尔量为Mg2++Al3+的总摩尔量的2倍。
所述步骤(3)搅拌速率为90~120rpm。
本发明的有益效果:
(1)本发明的硫化氢吸附剂为镁铝水滑石前躯体高温焙烧生成的焙烧态水滑石Mg1-xAlxOm,具有比表面积大、热稳定性高、抗烧结能力好的特点,铝镁金属离子可以达到分子和原子级的分散,很强的阴离子选择性,可以通过吸附水中的阴离子恢复层状结构;
(2)本发明的硫化氢吸附剂可在30℃~200℃的温度范围内吸附硫化氢气体,适用温度范围广;
(3)本发明的硫化氢吸附剂制备方法简单易行,吸附性能优越于活性炭,氧化铝等吸附材料,且成本低廉。
附图说明
图1为硫化氢吸附剂A1的XRD图谱。
具体实施方式
下面结合具体实施方式对本发明作进一步详细说明,但本发明的保护范围并不限于所述内容。
实施例1:本实施例的硫化氢吸附剂,化学式为Mg0.8Al0.2O1.1;
所述硫化氢吸附剂的制备方法,具体步骤如下:
(1)将镁盐(硝酸镁)和铝盐(硝酸铝)溶解于去离子水中得到混合盐溶液A;其中混合盐溶液A中Al3+的摩尔量与Mg2++Al3+的总摩尔量的比为0.2:1;
(2)配制混合碱溶液B,其中混合碱溶液B为氢氧化钠和碳酸钠的混合碱溶液,混合碱溶液B中OH-离子摩尔量为Mg2++Al3+的总摩尔量的2倍;
(3)在搅拌速率为90rpm条件下,将步骤(2)的混合碱溶液B与步骤(1)的混合盐溶液A分别逐滴滴入去离子水中使体系的pH值在9~9.5得到微乳液C;
(4)将步骤(3)的微乳液C置于温度为60℃条件下陈化反应16h,固液分离,固体水洗至中性,干燥、粉碎即得镁铝水滑石前躯体[Mg2+ 0.8Al0.2 3+(OH)2](CO3 2-)0.1·3H2O;
(5)将步骤(4)镁铝水滑石前躯体[Mg2+ 0.8Al0.2 3+(OH)2](CO3 2-)0.1·3H2O匀速升温至温度为500℃并恒温焙烧4h,研磨、筛分即得硫化氢吸附剂A1、A2、A3、A4、A5;
硫化氢吸附剂A1的XRD图谱见图1所示;
本实施例镁铝水滑石前躯体[Mg2+ 0.8Al0.2 3+(OH)2](CO32 -)0.1·3H2O,取5g本实施例的硫化氢吸附剂经研磨、筛分得到40~60目的硫化氢吸附剂A1、A2、A3、A4、A5放入固定床反应器中,在空速为3000h-1,混合气含有70%的N2和1000mg/m3的H2S条件下,当出口浓度高于进口浓度的95%时计算吸附容量;测得硫化氢吸附剂A1、A2、A3、A4、A5的吸附容量(见表1);
表1
从表1可知,硫化氢吸附剂A1、A2、A3、A4、A5的吸附容量均高达20mg/g左右。
本实施例的硫化氢吸附剂A1、A2、A3、A4、A5吸附饱和后,置于浓度为1mol/L的碳酸钠溶液中,浸泡12h后固液分离,固体沉淀置于温度为500℃焙烧5h即得再生硫化氢吸附剂A1、A2、A3、A4、A5;再生硫化氢吸附剂A1、A2、A3、A4、A5的吸附容量分别为18.9mg/g、 19.2mg/g、17.8mg/g、17.7mg/g、17.5mg。
实施例2:本实施例的硫化氢吸附剂,化学式为Mg0.72Al0.28O1.14。
所述硫化氢吸附剂的制备方法,具体步骤如下:
(1)将镁盐(硫酸镁)和铝盐(硫酸铝)溶解于去离子水中得到混合盐溶液A;其中混合盐溶液A中Al3+的摩尔量与Mg2++Al3+的总摩尔量的比为0.28:1
(2)配制混合碱溶液B,其中混合碱溶液B为氨水、碳酸氢钠和氢氧化钠的混合碱溶液,其中混合碱溶液B中OH-离子摩尔量为Mg2++Al3+的总摩尔量的2倍;
(3)在搅拌速率120rpm条件下,将步骤(2)的混合碱溶液B与步骤(1)的混合盐溶液A分别逐滴滴入去离子水中使体系的pH值在9.5~10.0得到微乳液C;
(4)将步骤(3)的微乳液C置于温度为70℃条件下陈化反应17h,固液分离,固体水洗至中性,干燥、粉碎即得镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·mH2O;(5)将步骤(4)镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·mH2O匀速升温至温度为450℃并恒温焙烧4h,研磨、筛分即得硫化氢吸附剂B1、B2、B3、B4、B5;
取5g本实施例的硫化氢吸附剂经研磨、筛分得到40~60目的硫化氢吸附剂B1、B2、B3、 B4、B5放入固定床反应器中,在空速为3000h-1,混合气含有70%的N2和1000mg/m3的H2S条件下,当出口浓度高于进口浓度的95%时计算吸附容量;测得硫化氢吸附剂B1、B2、B3、B4、B5的吸附容量(见表2);
表2
从表2可知,硫化氢吸附剂B1、B2、B3、B4、B5的吸附容量均高达33mg/g左右,本实施例的硫化氢吸附剂B1、B2、B3、B4、B5吸附饱和后,置于浓度为1mol/L的碳酸钠溶液中,浸泡12h后固液分离,固体沉淀置于温度为500℃焙烧5h即得再生硫化氢吸附剂B1、B2、 B3、B4、B5;再生硫化氢吸附剂B1、B2、B3、B4、B5的吸附容量分别为30.1mg/g、30.5mg/g、 29.5mg/g、27.6mg/g、30.3mg/g。
实施例3:本实施例的硫化氢吸附剂,化学式为Mg0.64Al0.36O1.18。
所述硫化氢吸附剂的制备方法,具体步骤如下:
(1)将镁盐(氯化镁)和铝盐(氯化镁)溶解于去离子水中得到混合盐溶液A;其中混合盐溶液A中Al3+的摩尔量与Mg2++Al3+的总摩尔量的比为0.34:1;
(2)配制混合碱溶液B,其中混合碱溶液B为碳酸钠、碳酸氢钠和氢氧化钠的混合碱溶液,其中混合碱溶液B中OH-离子摩尔量为Mg2++Al3+的总摩尔量的2倍;
(3)在搅拌速率为150rpm条件下,将步骤(2)的混合碱溶液B与步骤(1)的混合盐溶液A分别逐滴滴入去离子水中使体系的pH值在10.0~11.0得到微乳液C;
(4)将步骤(3)的微乳液C置于温度为80℃条件下陈化反应18h,固液分离,固体水洗至中性,干燥、粉碎即得镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·3H2O;(5)将步骤(4)镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·3H2O匀速升温至温度为500℃并分别恒温焙烧4h,研磨、筛分即得硫化氢吸附剂C1、C2、C3、C4、C5;
取5g本实施例的硫化氢吸附剂经研磨、筛分得到40~60目的硫化氢吸附剂C1、C2、C3、 C4、C5放入固定床反应器中,在空速为3000h-1,混合气含有70%的N2和1000mg/m3的H2S条件下,当出口浓度高于进口浓度的95%时计算吸附容量;测得硫化氢吸附剂C1、C2、C3、C4、C5的吸附容量(见表3);
表3
从表3可知,硫化氢吸附剂C1、C2、C3、C4、C5的吸附容量均高达45gm/g左右。
本实施例的硫化氢吸附剂C1、C2、C3、C4、C5吸附饱和后,置于浓度为1mol/L的碳酸钠溶液中,浸泡12h后固液分离,固体沉淀置于温度为500℃焙烧5h即得再生硫化氢吸附剂C1、C2、C3、C4、C5;再生硫化氢吸附剂C1、C2、C3、C4、C5的吸附容量分别为40.1mg/g、39.7mg/g、38.4mg/g、39.5mg/g、40.5mg/g。
Claims (5)
1.一种硫化氢吸附剂,其特征在于:化学式为Mg1-xAlxOm,其中0.2≤x≤0.34,2≤m≤6。
2.一种硫化氢吸附剂的制备方法,其特征在于,具体步骤如下:
(1)将镁盐和铝盐溶解于去离子水中得到混合盐溶液A;其中镁盐为硝酸镁、硫酸镁或氯化镁,铝盐为硝酸铝、硫酸铝或氯化铝;
(2)配制混合碱溶液B,其中混合碱溶液B为氨水、碳酸氢钠、氢氧化钠、碳酸钠的两种以上混合碱溶液;
(3)在搅拌条件下,将步骤(2)的混合碱溶液B与步骤(1)的混合盐溶液A分别逐滴滴入去离子水中使体系的pH值在9~11得到微乳液C;
(4)将步骤(3)的微乳液C置于温度为60~80℃条件下陈化反应16~18h,固液分离,固体水洗至中性,干燥、粉碎即得镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·mH2O;其中x为Al3+的物质量与(Mg2++Al3+)的总物质量的比值,0.2≤x≤0.34;m为结晶水数量,2≤m≤6;
(5)将步骤(4)镁铝水滑石前躯体[Mg2+ 1-xAlx 3+(OH)2]x+(CO3 2-)x·mH2O匀速升温至温度为450℃~650℃并恒温焙烧4~8h,研磨、筛分即得硫化氢吸附剂Mg1-xAlxOm。
3.根据权利要求2所述硫化氢吸附剂的制备方法,其特征在于:步骤(1)混合盐溶液A中Al3+的摩尔量与Mg2++Al3+的总摩尔量的比为(0.2~0.34):1。
4.根据权利要求2所述硫化氢吸附剂的制备方法,其特征在于:步骤(2)混合碱溶液B中OH-离子摩尔量为Mg2++Al3+的总摩尔量的2倍。
5.根据权利要求2所述硫化氢吸附剂的制备方法,其特征在于:步骤(3)搅拌速率为90~150rpm。
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