CN106944008A - 一种臭味吸附剂及其制备方法和用途 - Google Patents
一种臭味吸附剂及其制备方法和用途 Download PDFInfo
- Publication number
- CN106944008A CN106944008A CN201710230703.7A CN201710230703A CN106944008A CN 106944008 A CN106944008 A CN 106944008A CN 201710230703 A CN201710230703 A CN 201710230703A CN 106944008 A CN106944008 A CN 106944008A
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- China
- Prior art keywords
- stink
- coal
- adsorbent
- fusel oil
- ammonia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003463 adsorbent Substances 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 89
- 239000001760 fusel oil Substances 0.000 claims abstract description 58
- 239000003245 coal Substances 0.000 claims abstract description 53
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 44
- 239000000440 bentonite Substances 0.000 claims abstract description 33
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 33
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 33
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 29
- 239000011734 sodium Substances 0.000 claims abstract description 29
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- 239000002245 particle Substances 0.000 claims abstract description 27
- 235000020234 walnut Nutrition 0.000 claims abstract description 27
- RHZUVFJBSILHOK-UHFFFAOYSA-N anthracen-1-ylmethanolate Chemical compound C1=CC=C2C=C3C(C[O-])=CC=CC3=CC2=C1 RHZUVFJBSILHOK-UHFFFAOYSA-N 0.000 claims abstract description 25
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- 238000001035 drying Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 16
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- 238000002360 preparation method Methods 0.000 claims description 2
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- 239000010703 silicon Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 23
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- 240000007049 Juglans regia Species 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 20
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 11
- 238000001994 activation Methods 0.000 description 11
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 11
- 230000009965 odorless effect Effects 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 238000004587 chromatography analysis Methods 0.000 description 10
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 9
- 239000000463 material Substances 0.000 description 9
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- 229910052799 carbon Inorganic materials 0.000 description 4
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- 239000010865 sewage Substances 0.000 description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
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- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- XPDWGBQVDMORPB-UHFFFAOYSA-N Fluoroform Chemical compound FC(F)F XPDWGBQVDMORPB-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
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- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- BZORFPDSXLZWJF-UHFFFAOYSA-N N,N-dimethyl-1,4-phenylenediamine Chemical compound CN(C)C1=CC=C(N)C=C1 BZORFPDSXLZWJF-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical class [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 description 2
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- 238000006243 chemical reaction Methods 0.000 description 2
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- 229910052740 iodine Inorganic materials 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
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- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
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- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- 244000144730 Amygdalus persica Species 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
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- 238000011068 loading method Methods 0.000 description 1
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- 238000000746 purification Methods 0.000 description 1
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- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
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Abstract
本发明公开了一种臭味吸附剂及其制备方法和用途，该臭味吸附剂可作为煤制甲醇杂醇油臭味吸附剂使用，该臭味吸附剂采用膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳多种物质联合作用，发挥各自的特性相得益彰；颗粒均匀、比表面积大、微孔结构发达、孔径分布合理、毛细管丰富、吸附能力强，应用于煤制甲醇杂醇油除臭效果好；操作简单，生产成本低，处理效果好，无环境污染，可以重复利用。
Description
【技术领域】
本发明属于化工生产领域,具体涉及一种臭味吸附剂及其制备方法和用途。
【背景技术】
甲醇是一种基础化工原料，在化工、医药、轻纺等领域有着广泛的用途。甲醇可以用来直接合成含氧化工产品，主要用于制造甲醛、甲胺、二甲醚等一系列有机化工产品，而且还可以加入汽油掺烧或代替汽油作为动力燃料以及用来合成甲醇蛋白。在世界基础有机化工原料中，甲醇消耗量仅次于C2H4，C3H6和C6H6，居于第4位。煤制甲醇是煤化工项目的重要组成部分。通过煤制甲醇可以最大程度地缓解中国化工产业的发展与传统能源短缺之间的矛盾。我国煤炭资源丰富，发展煤制甲醇不仅合理利用了煤炭，而且可以减轻粗放式开采利用过程中对环境的污染破坏。
2015年我国煤制甲醇约2900万吨，同时产有58万吨杂醇油。在煤制甲醇工艺中，经蒸馏甲醇后剩余的杂醇油主要成分是甲醇、乙醇、丙醇、异丙醇、丁醇等，还含有异丁醇、2-丁醇、戊醇、异戊醇、2-戊醇、3-甲基-2-丁醇、2-甲基-1-丁醇、己醇、2-己醇、3-己醇、庚醇、2-庚醇、3-庚醇、2-甲基-1-己醇、2-乙基-1-戊醇、2-甲基-3-己醇等40多种化合物，其中还含有极少量的甲硫醇、乙硫醇、硫化氢等。由于含有极少量的硫化物，具有刺鼻难闻的臭味。由于硫化物的含量少，完全清除这种臭味困难，处理成本较高。目前煤制甲醇这些副产物杂醇油，大都没有经过认真、系统的回收和处理，或送入它系统裂解燃烧，或随残液直接排放，或简单处理后送进污水处理系统。其结果是既污染了环境，增大了污水处理系统负荷，又减少了企业的效益。
脱硫除臭的方法很多，对于不同的原料采用不同的方法处理。主要有物理吸附法、化学氧化法、生物分解法等。目前活性炭吸附法使用的最多，该方法运行操作方便，但是脱硫除臭精度不理想，很难满足环保要求。李芬等通过筛选载体，以氧化锌为活性组分，采用浸渍法制备出系列负载型氧化锌脱硫除臭剂，考察了浸渍氧化锌的活性炭除臭活性，并探讨了脱硫除臭剂的结构，期望寻求低成本高效的脱硫除臭材料用于环境中含硫恶臭污染物的治理(李芬，杨莹，姜蔚等，三种负载型氧化锌脱硫剂的除臭效能对比研究[J]，材料导报，2013，27(9)：97-99，103。)。窦燕生等利用氧化剂的氧化作用对粪便处理车间臭气物质进行氧化分解，以达到除臭或降低不快感的效果。在臭氧氧化作用下，在气相中除去硫化氢的效率比氨的效率高。在两个小时连续监测期间，硫化氢总去除率为88％，氨的总去除率为56.5％(窦燕生，洪燕峰，潘顺昌等，臭氧氧化法在粪便处理车间除臭的研究[J]，中国卫生工程学，2004，3(2)：70-72。)。赵鹏等探讨了生物法脱硫除臭的方法。恶臭气体生物脱臭原理是，在水、微生物和氧存在的条件下，利用微生物的代谢作用氧化分解发臭物质，以达到净化气体的目的。生物处理大致可以分为3个过程:发臭物质被载体(固定有微生物)吸附；发臭物质向微生物表面扩散、被微生物吸附；微生物将发臭物质氧化分解。不含氮的恶臭物质被分解成CO2和H2O，含硫恶臭物质被分解成S、SO3 2-、SO4 2-，含氮恶臭物质则被分解成NH4 +，NO2 -，NO3 -(赵鹏，栾金义，王京刚等，恶臭气体生物处理技术研究进展[J].化工环保.2005，25(1)：29-32。)。
对于来源不同的臭味，常采用不同的处理方法。上述方法主要是针对污水处理，动物的粪便、生活垃圾等。中国发明专利CN103708995A，2014.4.9公开了一种煤制甲醇的杂醇油脱硫除臭方法，通过向杂醇油中通入一定量的臭氧搅拌，之后加入硅藻土搅拌，过滤，即可得去除异味的杂醇油；中国发明专利CN 106187690A，2016.12.7公开了一种杂醇油臭味去除剂，该杂醇油臭味去除剂由明矾、硫酸锌、次氯酸钙、亚铝酸钠、硫酸钠、氧化锌、三氟甲烷磺酸钠和膨润土按照一定比例配比而成，上述两种技术方案均采用化学氧化和物理吸附结合的方法来去除杂醇油中的臭味，均用到了具有强氧化性的氧化剂，由于杂醇油的成分复杂，可能会使杂醇油中的某些组分被氧化而发生其他的副反应，进而对杂醇油除臭的效果产生影响。
【发明内容】
为解决上述问题，本发明提供一种臭味吸附剂及其制备方法和用途。
本发明的技术方案如下：一种臭味吸附剂，其特征在于：所述臭味吸附剂是由膨润土、硅藻土、腐植酸钠、无烟煤、核桃壳和硅溶胶组成。
进一步的，所述的臭味吸附剂，具有下列组成：
以上各组分质量百分比之和等于100％。
所述臭味吸附剂的制备方法:将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土8—25wt％、硅藻土12—36wt％、腐植酸钠6—17wt％、无烟煤13—29wt％和核桃壳18—40wt％混合，混合均匀后加入硅溶胶3—12wt％拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至200—1200℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
所述臭味吸附剂的用途：用于煤制甲醇杂醇油的臭味吸附。
活性炭是使用较广的一种除臭物质，具有比表面积大、吸附能力强等优点。缺点是不能全部去除臭味。采用多种吸附剂使之联合作用，效果会不会更好些？为了去除煤制甲醇杂醇油的刺鼻臭味，发明人使用了不同的吸附剂，如膨润土、硅藻土、无烟煤、腐植酸钠、核桃壳等，经过活化处理后使用。使用不同组分的吸附剂，可以发挥各自的特性相得益彰，去除煤制甲醇杂醇油的刺鼻臭味效果较好。
膨润土是一种粘土、主要化学成分是SiO2、Al2O3，还含有铁、镁、钙、钠、钾等元素。膨润土具有很好的吸附作用。膨润土的吸附既有膨润土与被吸附物质之间分子间引力，又有膨润土与被吸附物质之间的化学键力，还有膨润土与被吸附物质之间离子交换力等。
硅藻土是由硅藻的单细胞藻类死亡以后的硅酸盐遗骸形成的，主要成分是由无定形的SiO2组成，并含有少量Fe2O3、CaO、MgO、Al2O3及有机质。显微镜下可观察到天然硅藻土的特殊多孔性构造，这种微孔结构使硅藻土具有吸附性能强，消除异味的功能。硅藻土能够长时间消除异味和吸收、分解有害化学物质。
腐植酸钠是动植物遗骸埋藏在地底下，经过微生物亿万年的分解和转化，及一系列的化学过程积累起来的高分子有机物。其基本结构是芳环和脂环，环上连有羧基、羟基、羰基、醌基、甲氧基等官能团，具有良好的吸附、络合、交换、螯合等功能。
核桃壳是采用优质的山核桃壳作原料，经过破碎，过筛得到。核桃壳具有硬度高、耐磨损、抗压性好，化学性能稳定，不在酸碱中溶解、吸附截污能力强。核桃壳由于本身的硬度，理想的比重、多孔和多面性，具有很好的吸附性能。
无烟煤化学稳定性好，有棱角，近似于球体，具有足够的机械强度，良好的比表面积和化学稳定性，是非常优良的吸附剂。广泛应用于自来水厂、污水处理厂、化工、冶金、印染、食品、热电厂、造纸厂、制药厂、化肥厂、垃圾填埋厂、环保工程等。
硅溶胶属胶体溶液，无臭、无毒。硅溶胶为纳米级的二氧化硅颗粒在水中的分散液。硅溶液在失去水分时，单体硅酸逐渐聚合成高聚硅胶，随水分的蒸发，胶体分子增大，最后形成-SIO-O-SIO-薄膜。这种硅溶胶薄膜与膨润土共同把其它吸附剂颗粒相互粘合在一起，形成具有一定骨架的吸附剂。
由于膨润土本身的粘性，具有很好的粘接作用，与硅溶胶一起把其它颗粒粘合在一起，完全靠分子之间的亲和力和原料本身的特殊性质。由于采用多种优质材料，制成的臭味吸附剂比传统的一种原料的吸附剂如木质活性炭，或者煤质活性炭吸附性能更好。这种吸附剂孔径分布合理，达到最大吸附与脱附，从而大大提高了使用寿命。臭味吸附剂颗粒均匀、比表面积大、微孔结构发达、孔径分布合理、毛细管丰富、吸附能力强，应用于煤制甲醇杂醇油除臭效果特别好。
把制成的臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到无色无味的杂醇油。使用本发明的技术方案制得的臭味吸附剂处理煤制甲醇杂醇油，操作简单，处理效果好，生产成本低，无环境污染，可以重复利用。
本发明的有益效果是：本发明所要求保护的臭味吸附剂具有颗粒均匀、比表面积大、微孔结构发达、孔径分布合理、毛细管丰富、吸附能力强的优点；该臭味吸收剂具有一定的形状，便于过滤除去；该臭味吸附剂化学性质稳定，可应用于多个领域的除臭，应用于煤制甲醇杂醇油除臭效果特别好，可以把煤制甲醇杂醇油的臭味除去百分之九十九以上。
【具体实施方式】
下面结合具体实施方式对本发明作进一步的详细描述：
实施例1
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土17g、硅藻土16g、腐植酸钠6g、无烟煤15g和核桃壳38g混合，混合均匀后加入硅溶胶8g拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至800℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例2
煤制甲醇杂醇油臭味吸附剂的组成
把上述原料按要求粉碎成60—80目的颗粒，在混合机内分别加入膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳混合，混合均匀后加入硅溶胶拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至850℃。冷却，用5％次氯酸钙溶液蒸汽活化。
取100g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到12000ml无色无味的杂醇油。
实施例3
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土8g、硅藻土18g、腐植酸钠10g、无烟煤20g和核桃壳36g混合，混合均匀后加入硅溶胶8g拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至900℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例4
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土25g、硅藻土12g、腐植酸钠8g、无烟煤15g和核桃壳35g混合，混合均匀后加入硅溶胶5g拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至950℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例5
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土11g、硅藻土36g、腐植酸钠10g、无烟煤13g和核桃壳21g混合，混合均匀后加入硅溶胶9g拌和均匀，在成型机内做成30-40目(450--425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至810℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例6
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土21g、硅藻土25g、腐植酸钠6g、无烟煤24g和核桃壳18g混合，混合均匀后加入硅溶胶6g拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至910℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例7
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土14g、硅藻土18g、腐植酸钠17g、无烟煤18g和核桃壳30g混合，混合均匀后加入硅溶胶3g拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至820℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例8
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土10g、硅藻土15g、腐植酸钠15g、无烟煤27g和核桃壳21g混合，混合均匀后加入硅溶胶12g拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至830℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例9
臭味吸附剂的组成
将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土16g、硅藻土14g、腐植酸钠12g、无烟煤14g和核桃壳40g混合，混合均匀后加入硅溶胶4g拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至920℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
取50g煤制甲醇杂醇油臭味吸附剂装入层析柱中，加入煤制甲醇杂醇油层析，可得到5000ml无色无味的杂醇油。
实施例1-9制得的臭味吸附剂的去除臭味的效果评价：使用实施例1-9得到的臭味吸附剂对煤制杂醇油(硫化物含量2.25mg/ml)进行处理,并对处理后得到的煤制杂醇油中硫化物的含量进行检测。
经过郑州大学分析测试中心检测，煤制甲醇杂醇油处理前后结果对比如下：
表1煤制甲醇杂醇油处理前后结果对比
从上述数据可以看出，处理前煤制杂醇油中硫化物的含量是经实施例1-9处理后的煤制杂醇油中硫化物含量的一百多倍。也就是说使用本发明的方法，可以把煤制甲醇杂醇油的臭味除去百分之九十九以上。
本发明使用的硫化物的检测方法如下：
硫化氢的测定
原理：硫化氢被氢氧化镉-聚乙烯醇磷酸铵溶液吸收,生成硫化镉胶状沉淀,在硫酸溶液中,硫离子与对氨基二甲基苯胺和三氯化铁作用,生成亚甲基蓝,根据颜色深浅,用分光光度法比色测定。其化学反应如下:
H2S+Cd(OH)2→CdS↓+2H2O
吸收液：称取4.30g硫酸镉(CdSO4·8H2O),氢氧化钠0.30g溶于水。2种溶液混合后用水稀释至1000ml。此溶液为乳白色悬浮液,每次在使用前需要激烈振匀再取用。
对氨基二甲基苯胺溶液
贮备液：取25ml硫酸缓慢倒入15ml水中,放冷。称取6.00g对氨基二甲基苯胺盐酸盐[NH2C6H4N(CH3)2·2HCl]溶于以上H2SO4溶液中。可长期保存于冰箱中。使用液：吸取2.50ml贮备液，用1∶1的硫酸溶液稀释至100ml。
氯化铁溶液：称取50g三氯化铁(FeCl3·6H2O)溶于水中,稀释至50ml。若有沉淀需过滤后使用。
标准溶液：称取0.71g硫化钠晶体(Na2S·9H2O)溶于新煮沸冷却后的水中,稀释至100ml。标定后用新煮沸冷却后的水稀释成每ml含5μg的标准使用液。
标定方法：取20.00ml10.0100N的碘标准溶液置于200ml碘量瓶中,准确加入10.00ml硫化钠标准溶液,再加新煮沸冷却后的水80ml,立即加入5ml冰醋酸,混匀后在暗处放置2-3分钟；用0.0100N硫代硫酸钠标准溶液滴定至淡黄色，加入1ml新配制的0.5％淀粉呈蓝色，用少量水冲洗瓶内壁，再继续滴定至蓝色刚好消失为终点(此时有硫生成，使溶液微混浊，要特别注意终点颜色的突变)。记录所用硫代硫酸钠标准溶液的体积V(ml)，同时，另取10ml水，做空白滴定,其操作步骤同上。记录空白滴定所用硫代硫酸钠标准溶液的体积V0ml。
硫化氢(mg/ml)＝(V-V0)N·17/10
式中：V0———滴定空白时,消耗硫代硫酸钠的ml数；
V———滴定硫化氢贮备液时,消耗硫代硫酸钠溶液的ml数；
N———硫代硫酸钠标准溶液的当量浓度；
17———硫化氢的当量。
分析步骤
取100ml煤制甲醇重馏分加入10ml吸收液，充分摇振放置，每30min充分摇振一次，3个小时后显色分析。放置过程中应避免日光直接照射。
标准曲线的绘制
取7支25ml比色管,按下表配制标准色列:
表2标准曲线样品
以上各管分别加入1.5ml对氨基二甲基苯胺使用液,加盖混匀(不要振摇),放置1分钟,再加入1—2滴三氯化铁溶液,摇匀后排除Fe3+的颜色。用2cm比色皿,于波长760纳米处,以水为参比,测定吸光度(因试剂空白对温度敏感,易受分光度计中温度的影响,故以水为参比)。
按照上述方法，分别取木质活性炭、煤质活性炭、膨润土、硅藻土、煤制甲醇杂醇油臭味吸附剂(实施例1)处理后的煤制甲醇杂醇油测定其吸光度，计算出硫化氢的含量，见表3：
表3吸附剂对硫化氢的吸附
从上述数据可以看出，使用本发明公开的方法所制得的臭味吸附剂对硫化物进行处理的效果明显优于单一的具有吸附性的材料对硫化物的去除效果。故可进一步证明本发明相对于现有技术具有突出的实质性特点和显著进步。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种臭味吸附剂，其特征在于：所述臭味吸附剂是由膨润土、硅藻土、腐植酸钠、无烟煤、核桃壳和硅溶胶组成。
2.根据权利要求1所述的臭味吸附剂，其特征在于：
具有下列组成：
以上各组分质量百分比之和等于100％。
3.根据权利要求1所述的臭味吸附剂的制备方法，其特征在于:将膨润土、硅藻土、腐植酸钠、无烟煤和核桃壳粉碎成60—80目的颗粒，在混合机内分别加入膨润土8—25wt％、硅藻土12—36wt％、腐植酸钠6—17wt％、无烟煤13—29wt％和核桃壳18—40wt％混合，混合均匀后加入硅溶胶3—12wt％拌和均匀，在成型机内做成30-40目(450-425微米)的颗粒，装入烘干机烘干。装入钢管中在无氧环境下，加热至200—1200℃。冷却，用5％次氯酸钙溶液蒸汽活化,得臭味吸附剂。
4.根据权利要求1所述的臭味吸附剂的用途，其特征在于：用于煤制甲醇杂醇油的臭味吸附。
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