CN1176850C - 熔盐的生产方法及其用途 - Google Patents
熔盐的生产方法及其用途Info
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Abstract
本发明涉及一种用挤压机制造熔盐及其混合物的方法。原料被熔化并且发生反应,然后引导反应产物通过一个带碱金属盐的塔。
Description
本发明涉及通过挤压机制备盐熔融物及其混合物的方法,其中原料在该挤压机中被熔化并使其反应,随后使该反应产物经过一个含碱金属盐的塔。
挤压机一般用于熔化和混合聚合材料,如塑料。挤压机也可用作聚合物的反应器。例如,对于用于生产尼龙6的己内酰胺,已经描述了在挤压机中进行的阴离子聚合作用(B.VanBuskirk,M.K.Akkapeddi,Polym.Prepr.Vol.29,557(1988))。对于阴离子聚合反应,用挤压机替代罐式搅拌反应器的优点是容易处理高粘度物质。用挤压机还可以最佳地实现对完全混合参加反应的所有物质和良好传热的要求(G.Menges等人,New Polym.Mater.,Proc.Int.Semin.,129-148(1987))。在EP813904中,用挤压机装置制备药物活性组分。这里,带酸基的药物活性组分与熔融物中的碱反应。
盐熔融物,比如NaAlCl4,具有各种应用范围。盐熔融物可以用作蓄热器中的蓄热介质,比如在加热浴中作为传热介质用来覆盖和净化熔融金属,用于高熔点材料的电泳涂漆,或者在原电池中用作熔融电解质,如GB2046506描述的那样。这些盐的进一步可能的应用是可再充电钠电池。该盐可以用在工作温度在130℃和200℃之间的电池中(K.M.Abraham,D.M.Pasquariello,J.Electrochem.Soc.,Vol.137.1189-1190(1990))。
DE3419279描述了一种电化学电池,其中阴极基质浸入卤铝酸钠盐熔融电解质。
一个较新的应用领域是“ZEBRA电池”。这种高温电池由一个液态钠电极、一个beta-铝电解质和处在NaAlCl4熔融物的过渡金属氯化物的电极组成(B.Cleaver,V.S.Sharivker,J.Electrochem.Soc.,Vol.142,3409-3413(1995))。
DE3718920描述了通过向熔融物添加纯金属和碱金属卤化物来制备盐熔融物。反应电池在盐熔融物的熔点以上工作。在实施例中,碱金属卤化物是NaCl,熔化的碱金属是钠,隔板是β-氧化铝。由于使用纯钠,必须采取特殊的安全措施如在保护气体环境下工作。由于必须防止由形成的副产品AlHal3对隔板的污染,反应必须在单独的电池中进行。
为制备碱金属卤铝酸盐,已经描述了在一个密封管中进行的相应卤化铝和碱金属卤化物的反应(Friedmann,Taube,J.Am.Chem.Soc.,72,2236-2243(1950))。在该方法中,观察到压力增加到6-7大气压,这将引起难题(FR2168912)。该装置必须配备适当的安全保护。
迄今为止所公开的所有用于制备盐熔融物的方法都是间歇操作法。与连续制备过程相比,间歇方法具有一些严重缺陷。在更换批料期间,必须打开装置。那么产品会被周围空气中的氧气、水和灰尘玷污。更换批料导致设备停止运行,从而引起空时产率减小。一种有效的不连续过程要求大的装置。开机过程要求相应更多的能量和时间。已经发现,尤其是在设备启动期间,杂质会被引入该方法中。FR2168912描述了一种复杂的用于碱金属卤铝酸盐的净化过程。该两步净化过程由用来降解有机杂质的氧处理法和用于沉淀铁和重金属的铝处理法组成。铝处理法必须在氮气或氩气中进行。
本发明的目的是提供一种制备纯盐熔融物的连续方法,它排除了外界的不利影响,最大限度地减少了能量需求并且易于获得最佳空时产率。另一个目的是在尽可能短的时间内制造大量盐熔融物。
本发明的目的通过一种用于制备通式为MDHal(I)的盐熔融物及其混合物的方法来实现,
通式中,
M是锂、钠、钾、铷或铯,
D是铝,镓,铟或铊,和
Hal是氟,氯,溴或碘,
其特征在于,将原料即一种金属卤化物和一种碱金属卤化物熔化,然后在带有强制传输的可加热挤压机中进行连续反应或者,如果需要,进行不连续反应,随后使反应产物经过一含碱金属盐的塔。
加工出的产品适用作电化学电池中的熔融电解质、蓄热器中的蓄热介质,在加热浴中作为传热介质,例如,用来覆盖和净化熔化的金属用于电泳涂漆高熔点材料或作为可充电钠电池和原电池中的熔融电解质。
出人意料地,已经发现原料可以由一个挤压机处理。通过适当选择材料和滞留时间,能够避免由磨损引起的令人担忧的对产品的污染。
已经发现,在该方法中,可以省去在挤压机中由泵带动的强制传输,这明显地降低该方法对故障的敏感度。
任何显然适用于本领域技术人员的挤压机都可以用于该方法。尤其适用的挤压机是单螺杆挤压机,同向和反向旋转的多螺杆挤压机,排气式挤压机,行星齿轮挤压机,柱塞式挤压机和盘式挤压机。为了在挤压机中对盐进行处理,采用的物质的硬度及其化学特性体现了迄今还妨碍实施的特殊问题。通常,挤压机由钢制成。这种材料在盐的处理过程中会由于腐蚀和磨损而被严重损坏。
已经发现,在主要部件由镍合金制成的挤压机中,腐蚀可被明显地抑制。另外还发现,通过在与盐或其熔融物接触的挤压机的金属零件表面上涂敷本领域技术人员公知的材料如PTFE/PFA、瓷釉或陶瓷材料,可以保护这些零件不受腐蚀和磨损的侵害。为了减小磨损,可以在螺杆端部安装一个附加的轴承。
出人意料地,已经发现,尽管材料在挤压机中有非常短的几秒钟的平均滞留时间,安装带反流向的螺杆元件能够得到完全熔融和均匀的产品。
挤压机中的反应可以在大气氧气存在下或,如果需要,在保护气体气氛(如氮,二氧化碳或惰性气体)、在减压、大气压甚至超大气压下在50℃到800℃(在大气压下)的温度下进行。当在超大气压或减压下工作时,盐的熔点相应地变换,而且挤压机的加热阶段得到相应改变。
可以在低于原材料的升华温度下完成该方法。反应最好在升温下进行,因为在这种条件下盐的溶解度明显地较好。
在挤压机中处理盐期间,对加热阶段中温度的具体选择允许在处理过程中设置最佳温度程序。
为了实施该方法,使用的卤化铝是氟化物、氯化物、溴化物或碘化物,或者它们的混合物。合适的碱金属盐是锂、钠、钾、铷或铯的氟化物、氯化物、溴化物或碘化物,或其混合物。
本发明的一般示例在下文中被更详细地说明,并表示在附图中。图1示出带有固体计量装置2和下游塔3的可加热挤压机1。
为了制备符合通式(I)的盐及其混合物,通过固体计量装置2单独地将原料喂给挤压机。原料还可以先以相同比率进行预混合,然后通过一单独计量装置喂入。还可以在惰性气氛下装填挤压机。带有强制传输的挤压机推动盐床在螺槽中以1rpm到75rpm的螺杆速度向前运动。螺旋几何形状有3和25之间的1/d比率。在护套1的加热段,可以设置各种原料和成品的熔融温度。在最后的四分之一段,可以采用能引起返混的螺杆部件。这将增加该段的滞留时间,而且使还没有熔融的盐与液态熔融物混合。
由该方法生产的低粘度熔融物被喂给含对应碱金属盐的塔3。为了使残余量未反应的金属卤化物进行反应,使熔融物经过碱金属盐。
可以利用挤压机建立的传输压力将熔融物送到和经过塔。
为了更好地说明本发明,下面给出实施例,但是该实施例不适用于将本发明限制到其中公开的特征中。
实施例1:
NaAlCl4的制备
为了制备1kg/h NaAlCl4,经过固体计量装置将373.8g/h NaCl喂给一个挤压机,并经过另一个固体计量装置将626.2g/h AlCl3喂给该挤压机。一个带有强制传输的双螺杆挤压机以25rpm的螺杆速度在螺槽中将该盐床向前推进。可以改变外套的各种加热区,以便从喂料口向排出区伸展期间使盐达到它的熔点。在制备NaAlCl4中,喂给温度设为182℃。最后四分之一包括有反向传输方向的螺杆元件,从而在该区增加混合物的滞留时间。为了有助于更好地传热,将未熔化的盐与液体熔融物混合。
经过一个管道将形成的低粘度熔融物喂给含氯化钠颗粒床的塔。在塔里,未反应的AlCl3残渣转化为NaAlCl4。挤压机的传输压力足以输送熔融物到达并通过该塔而不需要额外的泵装置。
Claims (4)
1.通式为MDHal4(I)的盐熔融物及其混合物的制备方法,
通式中,
M是锂、钠、钾、铷或铯,
D是铝,镓,铟或铊,和
Hal是氟,氯,溴或碘,
其特征在于,通过一个固体计量装置喂给原料金属卤化物和碱金属盐,在带有强制传输的可加热挤压机(1)中熔化并反应,随后使反应产物经过一含有碱金属盐的塔(3)。
2.权利要求1的方法,其特征在于,在50℃和800℃之间的温度下,使原料在带有强制传输的可加热挤压机(1)中熔化并反应。
3.权利要求1或2的方法,其特征在于,该反应是在大气氧存在下或者,如果需要,在保护气体中在减压、大气压下或者超大气压下进行。
4.根据权利要求1的方法,其特征在于,该盐床是在一个挤压机中被处理,与盐或其熔融物接触的挤压机的零件由镍合金或涂有PTFE/PFA、瓷釉或陶瓷材料的金属制成,挤压机有一个1/d比率为3到25之间的的螺槽,螺杆速度在1rpm和75rpm之间。
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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DE19857788.5 | 1998-12-15 | ||
DE19857788A DE19857788A1 (de) | 1998-12-15 | 1998-12-15 | Verfahren zur Herstellugn von Salzschmelzen mit einem Extruder und deren Verwendung |
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CN1330613A CN1330613A (zh) | 2002-01-09 |
CN1176850C true CN1176850C (zh) | 2004-11-24 |
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CNB998145750A Expired - Fee Related CN1176850C (zh) | 1998-12-15 | 1999-12-03 | 熔盐的生产方法及其用途 |
Country Status (14)
Country | Link |
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US (1) | US6767665B1 (zh) |
EP (1) | EP1152982B1 (zh) |
JP (1) | JP2002532370A (zh) |
KR (1) | KR100569499B1 (zh) |
CN (1) | CN1176850C (zh) |
AT (1) | ATE295828T1 (zh) |
AU (1) | AU1970300A (zh) |
BR (1) | BR9916196A (zh) |
CA (1) | CA2355174A1 (zh) |
DE (2) | DE19857788A1 (zh) |
MX (1) | MX234882B (zh) |
MY (1) | MY130818A (zh) |
TW (1) | TW476734B (zh) |
WO (1) | WO2000035809A1 (zh) |
Families Citing this family (10)
Publication number | Priority date | Publication date | Assignee | Title |
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JP5237824B2 (ja) * | 2005-12-22 | 2013-07-17 | ヒェメタル ゲゼルシャフト ミット ベシュレンクテル ハフツング | アモルファスのフッ化セシウムアルミニウム錯体、その製造及び使用 |
CA2810068C (en) | 2010-09-03 | 2020-01-28 | Greg Naterer | Heat exchanger using non-pure water for steam generation |
WO2012139013A2 (en) * | 2011-04-06 | 2012-10-11 | Dow Global Technologies Llc | Apparatus, systems and methods for dispensing phase change material as liquid |
US10854929B2 (en) * | 2012-09-06 | 2020-12-01 | Field Upgrading Usa, Inc. | Sodium-halogen secondary cell |
CN104282955A (zh) * | 2013-07-09 | 2015-01-14 | 中国科学院上海硅酸盐研究所 | 制备可熔融电解质的方法及其装置 |
US9567232B1 (en) | 2015-08-20 | 2017-02-14 | General Electric Company | Method for preparing sodium chloro-aluminate |
RU2651200C2 (ru) * | 2016-04-04 | 2018-04-18 | Федеральное казенное предприятие "Государственный научно-исследовательский институт химических препаратов" (ФКП "ГосНИИХП") | Способ получения особо чистого безводного хлорида алюминия |
CN109097001B (zh) * | 2018-09-25 | 2021-03-19 | 中国科学院上海应用物理研究所 | 一种多组分氯化物共晶熔盐的制备方法 |
US11181325B2 (en) | 2019-12-23 | 2021-11-23 | Valgroup S.A. | System for the production of molten salt used as a heat transfer medium for a pyrolysis system |
CN114515559B (zh) * | 2021-11-05 | 2023-04-25 | 广州市鸿浩光电半导体有限公司 | 作用于电解炼铝时的氟铝酸钠晶体结晶系统及结晶方法 |
Family Cites Families (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3128151A (en) * | 1959-10-30 | 1964-04-07 | I C P M Ind Chimiche Porto Mar | Process for producing a sodium fluoaluminate composition having predetermined naf/alf3 ratio |
NL6509522A (zh) * | 1964-07-22 | 1966-01-24 | ||
ES365009A1 (es) * | 1968-03-21 | 1971-01-16 | Alloys And Chemical Corp | Un procedimiento para eliminar las impurezas del aluminio. |
US4141960A (en) * | 1968-09-03 | 1979-02-27 | Exxon Research & Engineering Co. | Complex bimetallic salts |
FR2168912A1 (en) | 1972-01-26 | 1973-09-07 | Rhone Poulenc Sa | Alkali haloaluminates prepn - prod used in metal sulphides and sulphoselenides prodn |
US3761578A (en) | 1972-03-09 | 1973-09-25 | S Anderson | Method of preparing purified lithium aluminum chloride |
CA1149865A (en) | 1979-08-22 | 1983-07-12 | Margaretha J. Nolte | Electrolyte for an electrochemical cell, and an electrochemical cell including the electrolyte |
DE3116469A1 (de) * | 1981-04-25 | 1982-11-11 | Kali-Chemie Ag, 3000 Hannover | Verfahren zur herstellung von kaliumtetrafluoroaluminat |
GB8613798D0 (en) * | 1986-06-06 | 1986-07-09 | Lilliwyte Sa | Electrolyte |
US5242669A (en) * | 1992-07-09 | 1993-09-07 | The S. A. Day Mfg. Co., Inc. | High purity potassium tetrafluoroaluminate and method of making same |
HU217858B (hu) * | 1995-01-24 | 2000-04-28 | Solvay Fluor Und Derivate Gmbh. | Eljárás forrasztópor és folyósítóanyag forrasztáshoz, valamint eljárás a forrasztópor előállítására |
-
1998
- 1998-12-15 DE DE19857788A patent/DE19857788A1/de not_active Withdrawn
-
1999
- 1999-12-03 AT AT99963385T patent/ATE295828T1/de not_active IP Right Cessation
- 1999-12-03 JP JP2000588079A patent/JP2002532370A/ja active Pending
- 1999-12-03 CN CNB998145750A patent/CN1176850C/zh not_active Expired - Fee Related
- 1999-12-03 AU AU19703/00A patent/AU1970300A/en not_active Abandoned
- 1999-12-03 KR KR1020017007457A patent/KR100569499B1/ko not_active IP Right Cessation
- 1999-12-03 US US09/857,602 patent/US6767665B1/en not_active Expired - Fee Related
- 1999-12-03 WO PCT/EP1999/009485 patent/WO2000035809A1/de active IP Right Grant
- 1999-12-03 DE DE59912078T patent/DE59912078D1/de not_active Expired - Fee Related
- 1999-12-03 CA CA002355174A patent/CA2355174A1/en not_active Abandoned
- 1999-12-03 EP EP99963385A patent/EP1152982B1/de not_active Expired - Lifetime
- 1999-12-03 BR BR9916196-6A patent/BR9916196A/pt not_active Application Discontinuation
- 1999-12-09 MY MYPI99005355A patent/MY130818A/en unknown
- 1999-12-09 TW TW088121596A patent/TW476734B/zh not_active IP Right Cessation
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2001
- 2001-06-14 MX MXPA01006056 patent/MX234882B/es not_active IP Right Cessation
Also Published As
Publication number | Publication date |
---|---|
DE19857788A1 (de) | 2000-06-21 |
KR20010101222A (ko) | 2001-11-14 |
ATE295828T1 (de) | 2005-06-15 |
KR100569499B1 (ko) | 2006-04-07 |
EP1152982B1 (de) | 2005-05-18 |
AU1970300A (en) | 2000-07-03 |
DE59912078D1 (de) | 2005-06-23 |
US6767665B1 (en) | 2004-07-27 |
CN1330613A (zh) | 2002-01-09 |
JP2002532370A (ja) | 2002-10-02 |
WO2000035809A1 (de) | 2000-06-22 |
EP1152982A1 (de) | 2001-11-14 |
MX234882B (en) | 2006-03-15 |
MY130818A (en) | 2007-07-31 |
CA2355174A1 (en) | 2000-06-22 |
TW476734B (en) | 2002-02-21 |
MXPA01006056A (es) | 2001-11-01 |
BR9916196A (pt) | 2001-09-04 |
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