CN1111507C - 硫酰氟的提纯方法 - Google Patents
硫酰氟的提纯方法 Download PDFInfo
- Publication number
- CN1111507C CN1111507C CN99108481A CN99108481A CN1111507C CN 1111507 C CN1111507 C CN 1111507C CN 99108481 A CN99108481 A CN 99108481A CN 99108481 A CN99108481 A CN 99108481A CN 1111507 C CN1111507 C CN 1111507C
- Authority
- CN
- China
- Prior art keywords
- purification
- hydrogen peroxide
- sulfuryl
- sulfuryl fluoride
- precursor
- 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.)
- Expired - Fee Related
Links
- 229910052731 fluorine Inorganic materials 0.000 title claims description 4
- 239000011737 fluorine Substances 0.000 title claims description 4
- 238000000746 purification Methods 0.000 title abstract description 12
- -1 sulfuryl fluorine Chemical compound 0.000 title 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 22
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000005935 Sulfuryl fluoride Substances 0.000 claims abstract description 10
- 239000002243 precursor Substances 0.000 claims abstract description 8
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 239000000460 chlorine Substances 0.000 claims abstract description 7
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 17
- 239000007789 gas Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 3
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract description 6
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000000361 pesticidal effect Effects 0.000 abstract 1
- 239000012264 purified product Substances 0.000 abstract 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 3
- 239000000575 pesticide Substances 0.000 description 3
- 230000002349 favourable effect Effects 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 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 150000003818 basic metals Chemical class 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000000266 injurious effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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)
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Removal Of Specific Substances (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
- Detergent Compositions (AREA)
Abstract
可用作例如杀虫剂的硫酰氟(SO2F2)通常含有制备条件下的氯、二氧化硫和其它酸性杂质。现已发现,将待提纯的硫酰氟与以水溶液形式存在的过氧化氢或其前体接触,能很有效地提纯硫酰氟。提纯后的产品令人惊异地适用于作为杀虫剂。
Description
技术领域
本发明涉及硫酰氟的提纯方法。
背景技术
硫酰氟(SO2F2)可用作杀虫剂。例如通过二氧化硫、氯或硫酰氯或氟化氢在一种催化剂如载于活性炭上的碱金属二氟化物上反应而制备它,这可参见DE-B 1 208 296。仍含有氟化氢、氯化氢、二氧化硫、氯和硫酰氯氟的粗产品在两个依次连接的洗涤器中借助水实现分离。
发明内容和具体实施方式
本发明的目的是,提供一种能有效提纯硫酰氟的方法。该目的通过这样一种方法达到,即一种制备提纯了的硫酰氟的方法,其中使含有选自二氧化硫、元素氟和氯中的一种或多种杂质的待提纯的硫酰氟与过氧化氢或其前体在0至40℃的一个温度下接触。
按本发明的方法,通过与过氧化氢或过氧化氢的前体接触而提纯硫酰氟。
“过氧化氢的前体”是指这些化合物,它能释放出过氧化氢,尤其是以其水溶液的形式释放。可使用的还包括这样的前体,它们不进行碱式反应(SO2F2分解的危险),例如过硼酸盐或过碳酸盐。优选与过氧化氢接触,它们以一种水溶液的形式存在是有利的。
水溶液中过氧化氢或其前体的浓度为0.1-10重量%是有利的。
待提纯的硫酰氟与提纯溶液的接触有利地在0至40℃的温度范围内进行。
按本发明的提纯方法可直接接在SO2F2的制备之后进行。变通地,按本发明的提纯方法可在时间上随应用场所延后进行。例如可将仍未或仅部分提纯的SO2F2在应用前、例如用作杀虫剂之前按本发明方法进行。当然,也可在SO2F2的制备与应用之间的任一时间来实施本发明的提纯方法。
按本发明的方法尤其可应用于提纯含有氯、氟和/或二氧化硫的硫酰氟。另外对还含有酸如氟化氢和/或盐酸的硫酰氟也有效。
除了其它优点外,本发明方法的一个优点在于,可迅速且有效地进行提纯,其中硫酰氟不会受到不利影响。
按本发明方法制备的硫酰氟基本上不含二氧化硫和氯,且可因此特别适用作杀虫剂。在使用之前,不必对它再作提纯。由于其纯度高,在应用它时,不必担心对敏感材料产生有害的影响。
下面的实施例用于解释本发明,而不对它的范围构成限制。实施例 用H2O2对SO2F2的提纯
含0.5%SO2(气相色谱测定的面积百分数)的SO2F2粗制气体在环境温度下被导入通过一个洗涤器,该洗涤器含有一种H2O2水溶液(H2O2浓度:8重量%)。从洗涤器流出的SO2F2含有少于0.05%(GC测定)的SO2。
Claims (4)
1.制备提纯了的硫酰氟的方法,其中使含有选自二氧化硫、元素氟和氯中的一种或多种杂质待提纯的硫酰氟与过氧化氢或其前体在0至40℃的一个温度下接触。
2.按权利要求1的方法,其特征在于,用过氧化氢的水溶液进行接触。
3.按权利要求1或2的方法,其特征在于,将过氧化氢或其前体配成水溶液,其浓度为0.1-10重量%。
4.按权利要求1的方法,其特征在于,提纯还另外含有选自HF和HCl中的一种或两种杂质的硫酰氟。
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19834882A DE19834882A1 (de) | 1998-08-01 | 1998-08-01 | Reinigung von Sulfurylfluorid |
| DE19834882.7 | 1998-08-01 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1243803A CN1243803A (zh) | 2000-02-09 |
| CN1111507C true CN1111507C (zh) | 2003-06-18 |
Family
ID=7876217
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99108481A Expired - Fee Related CN1111507C (zh) | 1998-08-01 | 1999-06-17 | 硫酰氟的提纯方法 |
Country Status (9)
| Country | Link |
|---|---|
| US (1) | US6143269A (zh) |
| EP (1) | EP0978478B1 (zh) |
| JP (1) | JP2000063107A (zh) |
| CN (1) | CN1111507C (zh) |
| AT (1) | ATE215049T1 (zh) |
| DE (2) | DE19834882A1 (zh) |
| DK (1) | DK0978478T3 (zh) |
| ES (1) | ES2173689T3 (zh) |
| PT (1) | PT978478E (zh) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10006247A1 (de) * | 2000-02-11 | 2001-08-16 | Solvay Fluor & Derivate | Disproportionierung von Sulfurylchlorfluorid |
| DE10111302A1 (de) * | 2001-03-09 | 2002-09-12 | Solvay Fluor & Derivate | Reinigung von Sulfurylfluorid |
| DE10204935A1 (de) * | 2002-02-07 | 2003-08-21 | Solvay Fluor & Derivate | Reinigung von Sulfurylfluorid |
| EP1571126A1 (de) * | 2004-03-04 | 2005-09-07 | Solvay Fluor GmbH | Reinigung von Sulfurylfluorid |
| CN101743997B (zh) * | 2008-12-12 | 2012-06-27 | 中国检验检疫科学研究院 | 一种熏蒸剂的复配方法及复配熏蒸剂 |
| CA3236324A1 (en) * | 2021-10-29 | 2023-05-04 | Joseph J. Pignatello | Method for scrubbing sulfuryl fluoride from a fluid |
| WO2023142027A1 (zh) * | 2022-01-29 | 2023-08-03 | 宁德时代新能源科技股份有限公司 | 一种制备硫酰氟的方法 |
| CN114368728B (zh) * | 2022-01-29 | 2022-11-08 | 宁德时代新能源科技股份有限公司 | 一种制备硫酰氟的方法 |
Family Cites Families (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB727062A (en) * | 1952-08-29 | 1955-03-30 | Nat Smelting Co Ltd | Improvements in or relating to the production of sulphuryl fluoride |
| US2875127A (en) * | 1955-03-07 | 1959-02-24 | Dow Chemical Co | Fumigation with sulfuryl fluoride |
| US3132925A (en) * | 1962-02-16 | 1964-05-12 | Stauffer Chemical Co | Method for production of sulfuryl fluoride |
| US3320030A (en) * | 1963-06-24 | 1967-05-16 | Allied Chem | Production of sulfuryl fluoride |
| US3403144A (en) * | 1964-01-15 | 1968-09-24 | Stauffer Chemical Co | Process for the preparation of sulfuryl fluoride |
| US3850542A (en) * | 1973-03-12 | 1974-11-26 | Dow Chemical Co | Treatment of chlorine-contaminated sulfuryl fluoride with unsaturated compounds |
| US4003987A (en) * | 1975-06-30 | 1977-01-18 | Texaco Development Corporation | Waste stream treatment |
| CA1066022A (en) * | 1975-07-02 | 1979-11-13 | Allied Chemical Corporation | Preparation of sulfur fluorides |
| 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 |
| DE19621516C2 (de) * | 1996-05-29 | 1998-11-05 | Angermeier S Schaedlingsbekaem | Verfahren zur Begasung eines Raumes mit Sulfurylfluorid |
-
1998
- 1998-08-01 DE DE19834882A patent/DE19834882A1/de not_active Withdrawn
-
1999
- 1999-06-17 CN CN99108481A patent/CN1111507C/zh not_active Expired - Fee Related
- 1999-07-27 DE DE59901044T patent/DE59901044D1/de not_active Expired - Fee Related
- 1999-07-27 ES ES99114236T patent/ES2173689T3/es not_active Expired - Lifetime
- 1999-07-27 EP EP99114236A patent/EP0978478B1/de not_active Revoked
- 1999-07-27 PT PT99114236T patent/PT978478E/pt unknown
- 1999-07-27 DK DK99114236T patent/DK0978478T3/da active
- 1999-07-27 AT AT99114236T patent/ATE215049T1/de not_active IP Right Cessation
- 1999-07-29 US US09/362,749 patent/US6143269A/en not_active Expired - Fee Related
- 1999-07-30 JP JP11217251A patent/JP2000063107A/ja not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| CN1243803A (zh) | 2000-02-09 |
| JP2000063107A (ja) | 2000-02-29 |
| ATE215049T1 (de) | 2002-04-15 |
| DE59901044D1 (de) | 2002-05-02 |
| EP0978478A1 (de) | 2000-02-09 |
| EP0978478B1 (de) | 2002-03-27 |
| DE19834882A1 (de) | 2000-02-03 |
| US6143269A (en) | 2000-11-07 |
| DK0978478T3 (da) | 2002-07-01 |
| PT978478E (pt) | 2002-07-31 |
| ES2173689T3 (es) | 2002-10-16 |
| HK1024224A1 (zh) | 2000-10-05 |
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Legal Events
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |