CN1223632A - 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 PDF

Info

Publication number
CN1223632A
CN1223632A CN97195934A CN97195934A CN1223632A CN 1223632 A CN1223632 A CN 1223632A CN 97195934 A CN97195934 A CN 97195934A CN 97195934 A CN97195934 A CN 97195934A CN 1223632 A CN1223632 A CN 1223632A
Authority
CN
China
Prior art keywords
fluorinated carboxylic
highly fluorinated
solution
carboxylic acids
recovery
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
Application number
CN97195934A
Other languages
English (en)
Other versions
CN1074407C (zh
Inventor
R·格拉斯伯格
R·A·苏尔兹巴奇
R·A·布兰登伯格
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dyneon GmbH
EIDP Inc
Original Assignee
Dyneon GmbH
EI Du Pont de Nemours and Co
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Priority claimed from DE1996131406 external-priority patent/DE19631406A1/de
Application filed by Dyneon GmbH, EI Du Pont de Nemours and Co filed Critical Dyneon GmbH
Publication of CN1223632A publication Critical patent/CN1223632A/zh
Application granted granted Critical
Publication of CN1074407C publication Critical patent/CN1074407C/zh
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • 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]

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

从气相中回收高氟化羧酸的方法
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。
CN97195934A 1996-08-05 1997-07-30 从气相中回收高氟化羧酸的方法 Expired - Fee Related CN1074407C (zh)

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 true CN1223632A (zh) 1999-07-21
CN1074407C 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)

* Cited by examiner, † Cited by third party
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
EP1570917B1 (en) * 2004-03-01 2009-06-10 3M Innovative Properties Company Method of coating a substrate with a fluoropolymer dispersion
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
GB0525978D0 (en) * 2005-12-21 2006-02-01 3M Innovative Properties Co Fluorinated Surfactants For Making Fluoropolymers
US7795332B2 (en) * 2005-07-15 2010-09-14 3M Innovative Properties Company Method of removing fluorinated carboxylic acid from aqueous liquid
US20080015304A1 (en) * 2006-07-13 2008-01-17 Klaus Hintzer Aqueous emulsion polymerization process for producing fluoropolymers
GB0514387D0 (en) * 2005-07-15 2005-08-17 3M Innovative Properties Co Aqueous emulsion polymerization of fluorinated monomers using a perfluoropolyether surfactant
GB0523853D0 (en) 2005-11-24 2006-01-04 3M Innovative Properties Co Fluorinated surfactants for use in making a fluoropolymer
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
US7754795B2 (en) * 2006-05-25 2010-07-13 3M Innovative Properties Company Coating composition
US20070276103A1 (en) * 2006-05-25 2007-11-29 3M Innovative Properties Company Fluorinated Surfactants
US8119750B2 (en) * 2006-07-13 2012-02-21 3M Innovative Properties Company Explosion taming surfactants for the production of perfluoropolymers
BRPI0807109A2 (pt) * 2007-02-16 2014-05-06 3M Innovative Properties Co Sistema e processo para a remoção de fluoroquiímicos da água
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

Family Cites Families (3)

* Cited by examiner, † Cited by third party
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
US4060535A (en) * 1976-08-31 1977-11-29 Tenneco Chemicals, Inc. Process for the production of metal salts of organic acids
EP0731081B1 (de) * 1995-03-09 1998-04-15 Dyneon GmbH Rückgewinnung hochfluorierter Carbonsäuren aus der Gasphase

Also Published As

Publication number Publication date
JP3937027B2 (ja) 2007-06-27
EP0938464B1 (de) 2002-07-31
RU2187495C2 (ru) 2002-08-20
ZA976919B (en) 1999-03-23
HK1020723A1 (en) 2000-05-19
CN1074407C (zh) 2001-11-07
EP0938464A1 (de) 1999-09-01
US6245923B1 (en) 2001-06-12
JP2001506966A (ja) 2001-05-29
WO1998005621A1 (de) 1998-02-12
CA2262702A1 (en) 1998-02-12

Similar Documents

Publication Publication Date Title
CN1074407C (zh) 从气相中回收高氟化羧酸的方法
CA1076517A (en) Process for the purification of electrolysis brine
US6228335B1 (en) Process for the production of sodium carbonate crystals
KR100929472B1 (ko) 염소 가스, 차아염소산 나트륨 수용액 및 액체 염소의 제조방법
US8900545B2 (en) Process for the production of high purity magnesium hydroxide
US4147761A (en) Hypochlorous acid process using sweep reactor
CN1076174A (zh) 从钠矿的盐水生产钠盐的方法
RO103830B1 (en) Separation and recovery method of chlorine
CA2032627C (en) Process for producing sodium carbonate and ammonium sulphate from sodium sulphate
US4328200A (en) Process for producing calcium hypochlorite
RU2134658C1 (ru) Безводный хлористый магний
US2224780A (en) Manufacture of crystalline magnesium hydroxide
JPH07790B2 (ja) 石炭の硫黄及び灰分の含有量を減少させる方法
JP2002527329A (ja) 硫酸アンモニウム精製方法
EP0005981B1 (en) Carbonation process for the manufacture of sodium bicarbonate
US4390512A (en) Process for producing calcium hypochlorite
JPH06263666A (ja) メタノールの製造方法
EP4273095A1 (en) Lithium bis(fluorosulfonyl)imide and method for preparing same, electrolyte and secondary battery
USRE31348E (en) Hypochlorous acid process using sweep reactor
RU2284298C1 (ru) Способ получения гранулированного хлорида кальция при комплексной переработке природных рассолов
JPS59176225A (ja) ジヒドロキシ芳香族化合物無水塩の製法
CN218793925U (zh) 一种硫酰氟制备产物分离收集系统
US20230387468A1 (en) Lithium bis(fluorosulfonyl)imide and preparation method thereof, electrolytic solution and secondary battery
FR2477126A1 (fr) Procede d'obtention d'un carbonate de magnesium de grande purete
US3983215A (en) Process for preparing NaOH.3.5 H2 O crystals

Legal Events

Date Code Title Description
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
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20011107

Termination date: 20110730