CN1284724C - 净化硫酰氟的方法 - Google Patents
净化硫酰氟的方法 Download PDFInfo
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- CN1284724C CN1284724C CNB038034743A CN03803474A CN1284724C CN 1284724 C CN1284724 C CN 1284724C CN B038034743 A CNB038034743 A CN B038034743A CN 03803474 A CN03803474 A CN 03803474A CN 1284724 C CN1284724 C CN 1284724C
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- Prior art keywords
- aluminum oxide
- adsorption step
- sulfuryl fluoride
- fluoride
- remove
- Prior art date
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- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 title abstract description 21
- 239000005935 Sulfuryl fluoride Substances 0.000 title abstract description 20
- 238000000746 purification Methods 0.000 title description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 13
- 238000001179 sorption measurement Methods 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000002594 sorbent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims 2
- 238000004140 cleaning Methods 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract 4
- LNKQQZFLNUVWQQ-UHFFFAOYSA-N 1-chloro-2,2-bis(4'-chlorophenyl)ethylene Chemical compound C=1C=C(Cl)C=CC=1C(=CCl)C1=CC=C(Cl)C=C1 LNKQQZFLNUVWQQ-UHFFFAOYSA-N 0.000 abstract 2
- 239000003795 chemical substances by application Substances 0.000 abstract 2
- 239000007789 gas Substances 0.000 description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 4
- 210000005239 tubule Anatomy 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- CNRIFWVXNQDPOX-UHFFFAOYSA-N S(=O)(=O)(Cl)Cl.[F] Chemical compound S(=O)(=O)(Cl)Cl.[F] CNRIFWVXNQDPOX-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- LSJNBGSOIVSBBR-UHFFFAOYSA-N thionyl fluoride Chemical compound FS(F)=O LSJNBGSOIVSBBR-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01B17/4561—Compounds containing sulfur, halogen and oxygen only
- C01B17/4576—Sulfuryl fluoride (SO2F2)
-
- 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
- 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
-
- 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
- B01D2253/104—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2256/00—Main component in the product gas stream after treatment
- B01D2256/26—Halogens or halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/206—Organic halogen compounds
- B01D2257/2066—Fluorine
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/302—Sulfur oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
由于生产和使用条件，硫酰氟可能掺杂有二氧化硫以及可能存在的其它杂质如SO2FCl。已被确定氧化铝作为吸附剂可以去除二氧化硫和如果存在也去除硫酰氯氟。额外地应用活性碳由此是多余的。
Description
本发明涉及从掺杂有二氧化硫的硫酰氟中获取净化的硫酰氟的生产方法。
硫酰氟是一种烟熏杀虫剂，例如可以在博物馆中应用。它可以用二氧化硫、氯和氟化氢通过催化剂生产出来。由于生产条件(也包括在其它的生产方法中)或者使用条件的限制，作为杂质可能含有二氧化硫。理想的是，如果把二氧化硫从由此掺杂的硫酰氟中去除出去。
美国专利4 950 464指出，可以用活化的氧化铝去除亚硫酰氟、酸性成分、水和某些其它的杂质。据所述美国专利称，用活性碳可以去除二氧化硫、氟化氢、氯化的烃和某些其它的杂质。所述吸附剂也可以先后使用。
本发明的任务是提供一种净化含有二氧化硫的硫酰氟的简便方法。
该任务通过本发明的方法得以解决。
根据本发明从掺杂有二氧化硫的硫酰氟中获取净化的硫酰氟的生产方法，为了去除二氧化硫，在一个吸附步骤中将掺杂有二氧化硫的硫酰氟与氧化铝接触。
优选使用活化的氧化铝。
可以使用任何形状的氧化铝，如颗粒或粉末。它用于吸附二氧化硫。若存在其它的杂质，如亚硫酰氟、酸性成分、水和硫酰氯氟，同样被吸附。不需要活性炭，特别是在不包含氯化的烃的生产条件下。因此优选不使用活性炭，只使用一种类型的吸附剂对于生产工艺技术当然是有利的。
当然也可以使用多个具有氧化铝的吸附步骤。运用一个氧化铝吸附步骤的根据本发明的净化方法当然也可以和常规的净化措施相结合，例如接触净化溶液，如水、弱碱性溶液，特别是弱碱性水溶液，或者氧化洗涤，例如过氧化氢水溶液。根据一个优选的实施形式，首先用氧化性洗涤，优选过氧化氢水溶液来接触硫酰氟，然后再把如此处理过的硫酰氟导入一个或多个氧化铝吸附步骤。
硫酰氟与氧化铝的接触，通常在-30℃至+100℃的温度范围内(优选环境温度)、压力范围在0至20巴(优选环境压力)下，特别是在气相中进行。
根据本发明方法的优点在于只需要使用一种吸附剂，即氧化铝，就可以可靠地去除二氧化硫和其它的杂质如硫酰氯氟。
下列实施例进一步解释了本发明，而并非将本发明局限在其范围之内。
所使用的Compalox(AN/V-850)是位于德国Bergheim的Martinswerk GmbH的一种商业产品。它是一种活性的粒状的氧化铝。
平均分析值： 90重量％Al2O3
灼热损耗： 9重量％
多孔体积： 0.35cm3/g
比表面积： 200-260m2/g
标准粒度： 5-10mm
堆密度： 850kg/m3
实施例1：
SO2F2的净化，高的SO2起始含量
在容量为250ml的玻璃管内填入200ml Compalox。在20℃和1巴的压力下将含有250ppm SO2的380克无水硫酰氟(SF)通过所述经填充的玻璃管。接触时间是3秒。通过Compalox后SO2的含量为100ppm。(分析方法：GC和Drger-测量小管SO2)
实施例2：
实验设计、实验流程、分析和使用量同实施例1。SO2的含量事先在H2O2洗涤剂中由250ppm减少到50ppm。
结果：
SO2初始量：50ppm
SO2最终量：32ppm
实施例3：
大实验，SO2起始含量较少
在100升的钢管中装入85千克Compalox。在20℃和1巴的压力下将含有25ppm SO2的418千克的无水硫酰氟(SF)通过所述经填充的钢管。接触时间是20秒。通过Compalox后SO2的含量为10ppm。(分析方法：GC和Drger-测量小管SO2)
实施例4：
精净化
运用实施例3中使用过的Compalox，在相同的物理条件下再通入含有10至15ppm SO2的SF 527千克。由于所加入的SF来自进行中的SF工艺流程，在生产的开始和后续步骤要抽取不同的样品。通过Compalox后SO2的含量在2到8ppm之间。(分析方法：GC和Drger-测量小管SO2)
Claims (7)
1.从掺杂有SO2的SO2F2中净化SO2F2的生产方法，其中为了去除SO2，在吸附步骤用氧化铝接触掺杂有SO2的SO2F2以除去SO2，所述吸附步骤中只包含氧化铝作为SO2的吸附剂。
2.根据权利要求1的方法，其特征在于，在吸附步骤之前和/或之后至少要经过一个用洗涤液接触SO2F2的步骤。
3.根据权利要求2的方法，其特征在于，在吸附步骤之前至少要经过一个用水、弱碱性液体或氧化性的液体接触SO2F2的步骤。
4.根据权利要求3的方法，其特征在于，在吸附步骤之前的清洗步骤包括使用过氧化氢水溶液。
5.根据权利要求1的方法，其特征在于，掺杂有SO2的SO2F2中还包含杂质SO2FCl，其在吸附步骤中用氧化铝接触以去除。
6.根据权利要求1的方法，其特征在于，氧化铝是活化的氧化铝。
7.根据权利要求1的方法，其特征在于，使吸附步骤排出的SO2F2再净化。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE10204935.1 | 2002-02-07 | ||
| DE10204935A DE10204935A1 (de) | 2002-02-07 | 2002-02-07 | Reinigung von Sulfurylfluorid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1628074A CN1628074A (zh) | 2005-06-15 |
| CN1284724C true CN1284724C (zh) | 2006-11-15 |
Family
ID=27618367
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB038034743A Expired - Fee Related CN1284724C (zh) | 2002-02-07 | 2003-01-30 | 净化硫酰氟的方法 |
Country Status (6)
| Country | Link |
|---|---|
| US (1) | US7014831B2 (zh) |
| EP (1) | EP1474358A1 (zh) |
| CN (1) | CN1284724C (zh) |
| AU (1) | AU2003208355A1 (zh) |
| DE (1) | DE10204935A1 (zh) |
| WO (1) | WO2003066520A1 (zh) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1571126A1 (de) * | 2004-03-04 | 2005-09-07 | Solvay Fluor GmbH | Reinigung von Sulfurylfluorid |
| KR101612145B1 (ko) | 2008-06-11 | 2016-04-12 | 아반트바이오 코포레이션 | 불화황 화합물의 브롬-촉진 합성 |
| CN102343210B (zh) * | 2011-09-28 | 2012-12-19 | 临海市利民化工有限公司 | 噻吩乙酸生产过程中产生的废氨气与烟气中so2的综合回收利用方法 |
| GB201116801D0 (en) | 2011-09-29 | 2011-11-09 | Johnson Matthey Plc | Purification process |
| CN106946231A (zh) * | 2017-03-30 | 2017-07-14 | 杭州茂宇电子化学有限公司 | 一种生产高纯度硫酰氟的方法及系统 |
Family Cites Families (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3320030A (en) * | 1963-06-24 | 1967-05-16 | Allied Chem | Production of sulfuryl fluoride |
| US4102987A (en) | 1975-09-25 | 1978-07-25 | The Dow Chemical Company | Process for preparing sulfuryl-fluoride and -chlorofluoride products |
| US3996029A (en) | 1975-09-26 | 1976-12-07 | The Dow Chemical Company | Purification of gases containing hydrogen fluoride impurity |
| DE3145012C2 (de) * | 1981-11-12 | 1986-07-24 | Bayer Ag, 5090 Leverkusen | Verfahren zur Reinigung Sulfurylfluorid enthaltender Abgase |
| US4950464A (en) * | 1989-02-10 | 1990-08-21 | The Dow Chemical Company | Purification of sulfuryl fluroide by selective adsorption |
| DE4343689C1 (de) * | 1993-12-21 | 1994-10-20 | Binker Materialschutz Gmbh | Verfahren und Vorrichtung zur Begasung eines Raumes mit Sulfurylfluorid |
| DE4441628C2 (de) | 1994-11-23 | 1998-06-18 | Binker Materialschutz Gmbh | Verfahren zur Begasung eines Raumes |
| KR100222918B1 (ko) * | 1997-09-04 | 1999-10-01 | 윤덕용 | γ-알루미나에 알칼리염 및 산화구리가 담지되어 있는 흡수제 |
| DE19834882A1 (de) * | 1998-08-01 | 2000-02-03 | Solvay Fluor & Derivate | Reinigung von Sulfurylfluorid |
| DE10005456A1 (de) * | 2000-02-08 | 2001-08-09 | Solvay Fluor & Derivate | Verfahren zur Rückgewinnung und/oder Abtrennung von Schwefeloxifluoriden aus Gasgemischen |
| DE10111302A1 (de) * | 2001-03-09 | 2002-09-12 | Solvay Fluor & Derivate | Reinigung von Sulfurylfluorid |
-
2002
- 2002-02-07 DE DE10204935A patent/DE10204935A1/de not_active Withdrawn
-
2003
- 2003-01-30 AU AU2003208355A patent/AU2003208355A1/en not_active Abandoned
- 2003-01-30 CN CNB038034743A patent/CN1284724C/zh not_active Expired - Fee Related
- 2003-01-30 WO PCT/EP2003/000917 patent/WO2003066520A1/de not_active Application Discontinuation
- 2003-01-30 EP EP03706401A patent/EP1474358A1/de not_active Withdrawn
-
2004
- 2004-08-06 US US10/912,573 patent/US7014831B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| DE10204935A1 (de) | 2003-08-21 |
| US20050022664A1 (en) | 2005-02-03 |
| US7014831B2 (en) | 2006-03-21 |
| AU2003208355A1 (en) | 2003-09-02 |
| CN1628074A (zh) | 2005-06-15 |
| EP1474358A1 (de) | 2004-11-10 |
| WO2003066520A1 (de) | 2003-08-14 |
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