CN1074407C - 从气相中回收高氟化羧酸的方法 - Google Patents
从气相中回收高氟化羧酸的方法 Download PDFInfo
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- CN1074407C CN1074407C CN97195934A CN97195934A CN1074407C CN 1074407 C CN1074407 C CN 1074407C CN 97195934 A CN97195934 A CN 97195934A CN 97195934 A CN97195934 A CN 97195934A CN 1074407 C CN1074407 C CN 1074407C
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- Prior art keywords
- fluorinated carboxylic
- highly fluorinated
- solution
- carboxylic acids
- recovery
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- 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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Treating Waste Gases (AREA)
Abstract
本发明涉及从废气流中回收高氟化羧酸的方法,其中,将废气流与密度大于1.15克/立方厘米的碱性洗涤溶液接触,以使高氟化羧酸的盐作为分离相分离出来,当碱性洗涤液是碳酸钾溶液时,是特别有利的。
Description
德国专利195 27 276(在1996,8月8日公开的专利说明书)涉及从废气流中回收高氟化羧酸的方法,其特征在于,将该废气与密度大于1.15克/立方厘米的碱性洗涤液接触,这样高氟化羧酸的盐作为分离相分离出。
作为该发明构思的一改进之处,已经发现所使用的碱性洗涤液宜为碳酸钾溶液。因此,本发明涉及从废气流中回收高氟化羧酸的方法,在该方法中,将该废气与密度大于1.15克/立方厘米的碱性洗涤液接触,这样高氟化羧酸的盐作为分离相沉淀出,其特征在于,所使用的碱性洗涤液是碳酸钾溶液。
当德国专利195 27 276中的碱性洗涤液是碱金属氢氧化物溶液时,如果欲净化的废气流包括二氧化碳,那么形成相应的碳酸盐。现在已经发现,当使用氢氧化钠溶液时,该碳酸钠导致涤气柱中结壳。此外,碳酸盐的形成伴随着所不希望的氢氧化钠的消耗。使用碳酸钾作为碱性试剂避免了这些缺陷。
如果使用碳酸钠代替碳酸钾,尽管没有氢氧化钠的消耗,但是显著地促进结壳形成。此外,碳酸钠具有低的溶解性。这表现在,在碳酸钠的情况下,具有该过程所需浓度的溶液的冷却由于过饱和导致沉淀。而碳酸钾不会出现这样的情况,所以可以不需要加热管线和容器。
已经进一步发现,当使用碳酸钾作为碱性试剂时,高氟化羧酸的钾盐以与使用氢氧化钾溶液相比更易于过滤出的形式离析出。除上述优点外,在使用碳酸钾时不会出现由于吸收的二氧化碳而大量消耗碱性试剂。
碱性洗涤溶液的密度有利地是1.2至1.4克/立方厘米。
关于进一步的详情参阅主专利DE-C-19527276。
现在借助于下面的实施例详细描述本发明。
实施例
在商业上可购得的长2000毫米、内径250毫米的涤气柱通入400Nm3/h的来自干燥粉状氟化聚合物过程的温度为171℃的废气。该废气包括750mg/Nm3(相当于300克/小时)的全氟辛酸。随着废气附加地从干燥器中将约20千克/小时的水带入洗涤过程中。涤气柱中的压力总计为约1巴绝对压力。
经喷嘴在涤气器中加入10平方米/小时的基本上由处于45℃的密度为1.30克/立方厘米的碳酸钾水溶液组成的碱性洗涤液。400Nm3/h的纯化废气流(现在仅包括0.8mg/Nm3的全氟辛酸,相当于0.32克/小时)从涤气柱的下部逸出。另外还存在水蒸汽,相当于在涤气器中的约45℃的温度下的水分压。
以平行流的方式操作涤气器。碱性洗涤介质和所产生的全氟辛酸的钾盐从涤气柱直接流入体积为0.4立方米的分离容器中,在这里不溶于碱性洗涤溶液的全氟辛酸的钾盐漂浮到顶部形成糊状层。从分离器的底部抽出现在实际上不包含全氟辛酸的钾盐的碱性洗涤溶液,并泵送回洗涤柱。在洗涤介质中溶解的全氟辛酸的钾盐的浓度是约170毫克/升。通过加入碳酸钾使洗涤液的密度保持在所希望的约1.30克/立方厘米的值。分离出作为糊状层的全氟辛酸的钾盐经分离器的溢流口与一些洗涤介质一起流入罐中。通过非常缓慢的搅拌器帮助排出过程,该搅拌器直接浸入上层中。在分离容器中,洗涤溶液和所形成的全氟辛酸钾泡沫的分离是非常好的。
在几个小时放置之后,再一次在罐中分离成二相:基本上由剩余的洗涤液组成的下层相和糊状上层相。分离出下层相,并使之循环回洗涤过程中。
糊状上层相包含36重量%的全氟辛酸钾。
可以进一步加工在该方法中获得的浓缩液以得到纯的100重量%的全氟辛酸。
值得一提的是,虽然在该方法中获得的浓缩液是可搅拌和可泵送的混合物,但是它不是全氟辛酸钾盐的稳定溶液。为了获得稳定的溶液,必须加入更多的水。然而,这对于进一步加工不是绝对需要的。
因为已经分离的下层相循环回上述洗涤过程中,所以无全氟辛酸的损失。在操作几周之后未发现由于柱中结壳所造成的洗涤过程的损坏。
Claims (1)
1、从废气流中回收高氟化羧酸的方法,其中,将废气流与密度大于1.15克/立方厘米的碱性洗涤溶液接触,以使高氟化的羧酸的盐作为分离相分离出来,其特征在于所使用的碱性洗涤液是碳酸钾溶液。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19631406.2 | 1996-08-05 | ||
DE1996131406 DE19631406A1 (de) | 1995-07-26 | 1996-08-05 | Rückgewinnung hochfluorierter Carbonsäuren aus der Gasphase |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1223632A CN1223632A (zh) | 1999-07-21 |
CN1074407C true CN1074407C (zh) | 2001-11-07 |
Family
ID=7801711
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN97195934A Expired - Fee Related CN1074407C (zh) | 1996-08-05 | 1997-07-30 | 从气相中回收高氟化羧酸的方法 |
Country Status (9)
Country | Link |
---|---|
US (1) | US6245923B1 (zh) |
EP (1) | EP0938464B1 (zh) |
JP (1) | JP3937027B2 (zh) |
CN (1) | CN1074407C (zh) |
CA (1) | CA2262702A1 (zh) |
HK (1) | HK1020723A1 (zh) |
RU (1) | RU2187495C2 (zh) |
WO (1) | WO1998005621A1 (zh) |
ZA (1) | ZA976919B (zh) |
Families Citing this family (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7279522B2 (en) * | 2001-09-05 | 2007-10-09 | 3M Innovative Properties Company | Fluoropolymer dispersions containing no or little low molecular weight fluorinated surfactant |
ITMI20021581A1 (it) * | 2002-07-18 | 2004-01-19 | Ausimont Spa | Procedimento di abbattimento di tensioattivi anionici fluorurati |
JP2004065970A (ja) * | 2002-07-22 | 2004-03-04 | Toshio Hayashi | 調理用補助具 |
DE602004021467D1 (de) * | 2004-03-01 | 2009-07-23 | 3M Innovative Properties Co | Verfahren zum Beschichten eines Gegenstands mit einer fluorhaltigen Kunststoffsdispersion |
US7138551B2 (en) * | 2004-11-05 | 2006-11-21 | E. I. Du Pont De Nemours And Company | Purification of fluorinated alcohols |
GB2427170A (en) * | 2005-06-17 | 2006-12-20 | 3M Innovative Properties Co | Fluoropolymer film having glass microspheres |
GB0514398D0 (en) * | 2005-07-15 | 2005-08-17 | 3M Innovative Properties Co | Aqueous emulsion polymerization of fluorinated monomers using a fluorinated surfactant |
US7671112B2 (en) | 2005-07-15 | 2010-03-02 | 3M Innovative Properties Company | Method of making fluoropolymer dispersion |
GB0514387D0 (en) * | 2005-07-15 | 2005-08-17 | 3M Innovative Properties Co | Aqueous emulsion polymerization of fluorinated monomers using a perfluoropolyether surfactant |
GB0525978D0 (en) * | 2005-12-21 | 2006-02-01 | 3M Innovative Properties Co | Fluorinated Surfactants For Making Fluoropolymers |
GB0523853D0 (en) | 2005-11-24 | 2006-01-04 | 3M Innovative Properties Co | Fluorinated surfactants for use in making a fluoropolymer |
US20080015304A1 (en) | 2006-07-13 | 2008-01-17 | Klaus Hintzer | Aqueous emulsion polymerization process for producing fluoropolymers |
GB2430437A (en) * | 2005-09-27 | 2007-03-28 | 3M Innovative Properties Co | Method of making a fluoropolymer |
US7728087B2 (en) | 2005-12-23 | 2010-06-01 | 3M Innovative Properties Company | Fluoropolymer dispersion and method for making the same |
US20070276103A1 (en) * | 2006-05-25 | 2007-11-29 | 3M Innovative Properties Company | Fluorinated Surfactants |
US7754795B2 (en) * | 2006-05-25 | 2010-07-13 | 3M Innovative Properties Company | Coating composition |
US8119750B2 (en) * | 2006-07-13 | 2012-02-21 | 3M Innovative Properties Company | Explosion taming surfactants for the production of perfluoropolymers |
EP2132143B1 (en) * | 2007-02-16 | 2012-12-26 | 3M Innovative Properties Company | System and process for the removal of fluorochemicals from water |
US20080264864A1 (en) * | 2007-04-27 | 2008-10-30 | 3M Innovative Properties Company | PROCESS FOR REMOVING FLUORINATED EMULSIFIER FROM FLUOROPOLMER DISPERSIONS USING AN ANION-EXCHANGE RESIN AND A pH-DEPENDENT SURFACTANT AND FLUOROPOLYMER DISPERSIONS CONTAINING A pH-DEPENDENT SURFACTANT |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2432473A1 (de) * | 1974-07-06 | 1976-01-22 | Hoechst Ag | Verfahren zur herstellung saurer salze niederer fettsaeuren und halogenfettsaeuren |
CN1137514A (zh) * | 1995-03-09 | 1996-12-11 | 赫彻斯特股份公司 | 从气相中回收高氟化羟酸的方法 |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4060535A (en) | 1976-08-31 | 1977-11-29 | Tenneco Chemicals, Inc. | Process for the production of metal salts of organic acids |
-
1997
- 1997-07-30 JP JP50757898A patent/JP3937027B2/ja not_active Expired - Fee Related
- 1997-07-30 WO PCT/EP1997/004146 patent/WO1998005621A1/de active IP Right Grant
- 1997-07-30 US US09/214,456 patent/US6245923B1/en not_active Expired - Lifetime
- 1997-07-30 EP EP97940048A patent/EP0938464B1/de not_active Expired - Lifetime
- 1997-07-30 RU RU99104514/04A patent/RU2187495C2/ru not_active IP Right Cessation
- 1997-07-30 CA CA002262702A patent/CA2262702A1/en not_active Abandoned
- 1997-07-30 CN CN97195934A patent/CN1074407C/zh not_active Expired - Fee Related
- 1997-08-04 ZA ZA976919A patent/ZA976919B/xx unknown
-
1999
- 1999-12-21 HK HK99105999A patent/HK1020723A1/xx not_active IP Right Cessation
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2432473A1 (de) * | 1974-07-06 | 1976-01-22 | Hoechst Ag | Verfahren zur herstellung saurer salze niederer fettsaeuren und halogenfettsaeuren |
CN1137514A (zh) * | 1995-03-09 | 1996-12-11 | 赫彻斯特股份公司 | 从气相中回收高氟化羟酸的方法 |
Also Published As
Publication number | Publication date |
---|---|
EP0938464B1 (de) | 2002-07-31 |
US6245923B1 (en) | 2001-06-12 |
WO1998005621A1 (de) | 1998-02-12 |
JP3937027B2 (ja) | 2007-06-27 |
ZA976919B (en) | 1999-03-23 |
HK1020723A1 (en) | 2000-05-19 |
CA2262702A1 (en) | 1998-02-12 |
JP2001506966A (ja) | 2001-05-29 |
CN1223632A (zh) | 1999-07-21 |
EP0938464A1 (de) | 1999-09-01 |
RU2187495C2 (ru) | 2002-08-20 |
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Granted publication date: 20011107 Termination date: 20110730 |