CN1080039A - 真空或致冷装置绝热套抽真空的改进方法 - Google Patents
真空或致冷装置绝热套抽真空的改进方法 Download PDFInfo
- Publication number
- CN1080039A CN1080039A CN92113646A CN92113646A CN1080039A CN 1080039 A CN1080039 A CN 1080039A CN 92113646 A CN92113646 A CN 92113646A CN 92113646 A CN92113646 A CN 92113646A CN 1080039 A CN1080039 A CN 1080039A
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- Prior art keywords
- getter
- vacuum
- inner space
- container
- pump
- Prior art date
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Images
Classifications
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Abstract
用于真空瓶绝热套抽真空的改进方法,真空瓶有
内壁,外壁,和由这两个壁形成的内层空间,它全部或
部分地填入绝缘材料,还有吸湿剂和吸气剂。吸湿剂
是一种化学干燥剂。
Description
本发明涉及对绝热套,特别是真空瓶或其他致冷装置的外套抽真空的改进方法,这种致冷装置例如用于贮存和/或输送低温气体诸如氮、氧、氢、氦、氩等或其他需要保持温度不同于室温,通常是低于室温的物质的专用管道。众所周知,所述外套的绝缘效果是利用真空和绝缘材料获得的。
本发明的新方法特别优越的地方是,它可使所述外套在很短的时间内达到工作状态。
根据一般的实践经验,为了达到上述目的都是使用带有真空套的真空瓶或管道来获得适当的绝热效果。作为进一步的绝热措施,通常在外套中放入绝缘材料,例如玻璃棉,多孔有机聚合物(例如,聚氨酯和各种成份的树脂),而最常用的是所谓“多层”的物质。后者是由有机聚合物(例如聚烯烃)板和涂铝塑料交替叠合而成,上述聚合物最好具有交联结构,涂铝塑料则是由例如真空气相沉积法将铝涂覆在塑料薄膜上而得到的。
大家也知道,在所述外套中,真空有随着时间而恶化的趋势,这是因为内部组分,甚至套壁有释气作用(即散发出气体物质如CO,N2,H2,H2O,O2等)和由于可能的“泄漏”(即大气渗入)引起的。为了保持真空,通常将吸收气体的材料放入外套中,这种材料一般由沸石,分子筛,硅胶,活性炭(木炭)和其他具有物理作用的吸气材料组成。这些物质必须保持在很低的温度下,例如液氮温度或更低的温度下,以便能吸收大部分这类气体物质。然而,上述的物理吸气材料并不能有效地吸收氢。因此,正如GB-A-921273所述那样,需要在外套中放入,例如氧化钯。根据反应:
事实上氧化钯将氢转化为水。
水再被沸石吸收,或者被外套中的其他物理吸附剂所吸收。
使用这些方法带来的第一个缺点是真空瓶或上述管道绝缘套的准备需要很长的时间,因为物理吸附剂(沸石等)的活化需要在泵的作用下进行长时间的热处理,这可能要持续几天。
这一过程的长短主要取决于需要将物理吸附剂和绝缘材料中残存的水量尽可能地减小到什么程度。大大地提高系统热处理的温度(例如,超过150°~200℃)可使时间缩短一些,但这种处理往往不能进行,因为所牵涉到的材料不适用于这样的温度,或者因为一些实际的原因或不得不考虑过程经济性之故。
第二个缺点来自吸附作用的物理本质,它使反应变成可逆的。因此,例如,当真空瓶放空和其内部温度为室温时,被吸收的气体会重新逸出,使外套内的压力升高。结果,在填充已经回复至室温的内容器(真空瓶或管道)的过程中会观察到强烈的沸腾现象,并有气体损失,这是由于绝缘条件恶化造成的。经过一定时间之后,一旦沸石冷却至低温温度,并再次吸收气体时,绝缘作用又再次出现。这个问题称为“汽化”,它是一个严重的问题,特别是在液化气体如H2和He的情况下,一般这些气体较昂贵,而且蒸发热较低。还要指出一点,现用的一些已知材料会与液化气体起作用,只要容器内部有泄漏,例如,因为有裂缝,则这些材料就可能偶而与它们接触。特别是PdO不能与液化H2一起用,因为在内壁有破损的情况下可能会引起爆炸。在液态O2的情况下,当使用活性炭(木炭)时也会发生同样的事情。
C.波菲托等人在真空科学工业杂志A5(6),3442,(1987)中建议采用GB-A-2043691公开的基于Zr-V-Fe合金的吸气材料。这种材料的确能解决上面提到的一些问题,因为从化学上来说它能吸收导致真空恶化的各种气体,特别是氢。
然而,在制造过程中,绝缘材料会导致水大量释出,这会在整个装置工作过程中严重影响对其他气体物质的吸收效率。
因此,本发明的第一个目的就是提供一种,能缩短准备真空瓶或其他例如贮存和/或输送液化气体的致冷装置的绝缘套和对其抽真空所需的时间的方法。
本发明的另一个目的是要提供一种如上面所述的方法,它在容器一旦排空和回复至室温之后,在用液化气体充填容器过程中不会产生“汽化”问题。
本发明还有一个目的是要提供一种可消除使用某些维持真空的材料特别是氧化钯和活性炭(木炭)时带来的麻烦的方法。这些材料实际上会分别与氢和氧起作用,引起爆炸,假如两种气体中的任一种处于液态,置于绝缘的容器内,并且如果这个容器有破损的话。
本发明还有一个目的是要提供一种能获得一种绝缘装置(真空瓶或管道)的方法,这种装置在其整个工作过程中,能在化学上高效地抽吸不希望的气体。
这些目的可以通过改进抽真空和制作绝热套,特别是真空瓶或另一种致冷装置的外套的方法来达到,这种致冷装置通常具有内壁和外壁,内外壁之间的内层空间全部或部分地填入绝缘材料,该内层空间还贮存着吸湿剂和吸气剂,其特点是,这种吸湿剂是一种化学干燥剂,最好选用H2O蒸汽压低于1帕(Pa)的吸附剂,特别是氧化钡,氧化锶,五氧化二磷及它们的混合物。
根据最佳的,非常有效的实施例,新方法包含下列连续的步骤:
A.外套的内层空间首先用真空泵抽真空至压力低于100帕(Pa);
B.该内层空间中同时受到所述的化学干燥剂的作用,而吸气剂则保持在非激活状态;
C.所述内层空间进一步用真空泵抽真空至压力低于5帕(Pa);
D.激化所述的吸气剂;
E.通过切断泵与外套内层空间之间的连接而使外套与泵分开。
有时,上述A项的泵抽真空在进行B项时可以停止,在进行A项和B项时,所述真空瓶或另一种致冷装置的内壁可以是热的,温度不超过150℃,最好是120℃,这样可促使风从绝缘材料中释出。
B项操作正常情况下持续不超过48小时,最好是2至48小时,而过去却需要几天。
另外,与现有技术不同,所述化学干燥剂和吸气剂最好放在隔开的区域内,贴着所述真空瓶或其他致冷装置的外壁。
对于所述吸气剂,它要以由能在较低温度下激活的合金构成,如钡和/或锆基合金,最好是Ba-Li合金,这点已在用同一申请人名字发表的欧洲专利申请No.92830186中公开过,特别希望采用具有原始分子式为BaLi4的合金。
更详细地说,这种改进的新方法允许对致冷装置(真空瓶,输送管道等)的绝热套进行抽真空,并使之适合于贮存和/或输送温度必须保持在不同于室温,特别是低于室温的材料。这种方法可以借助特殊的(化学的)吸水剂和吸气剂的共同作用,吸收在本过程和致冷装置连续工作过程中产生的气体。通常,吸水剂是在过程的第一阶段起作用(提供可加速本过程的“原地”吸水作用),而吸气剂只是在下一阶段才被激活,它通常是对不是水的其他一些气体,例如O2,N2,CO,H2等起化学吸附剂的作用。
下面参照附图更清楚地说明本发明,附图仅起说明作用,并不以任何方式限制本发明的应用范围,其中:
图1表示具有根据本发明的绝缘套的、用于贮存液化气体的常用金属真空罐的横截面的示意图;
图2表示用图1的真空罐进行试验的结果的曲线图;
图3表示在真空套内,干燥剂与吸气剂的最佳配置方案。
下面参照类似图1所示的真空罐的容器说明应用本发明方法的一系列操作,但是,同样的操作也可适用于输送液化气体的绝缘管道。
大家知道,真空罐1含有一个内桶或容器2,它最好是由金属,例如钢制成,形成一个适合于贮存液化气体的内部容积或有用空间3,液化气体通过“颈部”6与外界相通,正常情况下,颈部6是封闭的,但不密封。外壁或罩套4与内壁2一起形成一个套5,它部分地,至少是在围绕内壁2的部分填入绝缘材料9,这种绝缘材料最好是上面提到的“多层”形式的。套5通过接头8和阀7用于切断或断开与泵的连接。
根据本发明,在套5中放有化学吸湿剂10和吸气剂11,它们位于隔开的不同区域,贴近外壁4,这与现有技术相反,后者吸气剂放在温度最低的贴近内壁的地方。然后,套5的第一个泵吸步骤开始,通过管接头8对其抽真空,直到压力为100帕(Pa)或更低,这只需要几分钟。接着,阀7关闭,使容器与泵吸装置断开,同时吸水剂10在2至48小时的时间内,对从绝缘材料9释出的水蒸汽发挥选择性的抽吸作用。
在这个步骤过程中,阀7也可以在上述抽吸时间内保持打开。然而,在这种情况下,干燥剂10总是吸收大部分水蒸汽,因为泵的作用受到连接管接头8的流导的限制。再者,在吸收水蒸汽的这个阶段(利用或不利用从外部的泵吸作用),例如可通过向空间3输入热空气或热水使内壁2均匀加热到不超过150℃,以便加速除去水蒸汽绝缘材料9,特别是贴近壁2的最里层中的水蒸汽。
在抽吸时间过后,重新打开阀7(假如它已被关断的话),泵吸作用再次开始,使压力降至5帕(Pa)或更低。这时,吸气剂11例如可通过一个发热装置而激活,这个发热装置安放在外面与吸气剂的内部位置相对应的位置上。可以简单地使用火焰,热空气枪,电阻或其他类似方法进行加热。所达到的温度取决定于所选用的吸气剂类型。最好使用能够在低的或很低的温度下激活的吸气剂,例如在欧洲专利申请No.92830186中公布的Ba-Li合金,根据同一申请人的欧洲专利申请No.92830185,这种合金放入一个装有热伸缩盖的泡囊中。这种吸气剂不需要在高于120℃的温度下加热而激活。
有时,在本方法的最后阶段,关闭阀7,使管接头8相应地与泵隔离并密封起来(例如,通过“关断作用”)而使套5和外界完全隔离。
如果被吸收的气本不含水,则同样的吸气剂工作要好得多。这就是为什么建议首先使气体与效力强大的干燥剂例如BaO接触,然后再在单独的区域内与吸气剂,例如BaLi4接触的理由。
更详细地说,根据图3的实施例,所述化学干燥剂10和所述吸气剂11可以安放在容器12内,该容器被一多孔隔板13分隔成内区和外区,内区14含有所述吸气剂,外区15与含有绝缘材料9的空间相通。并含有所述化学干燥剂10,它可防止水蒸汽穿过所述隔板而流向吸气剂11。
容器12可以为一个带有上开口和平的(例如,水平的)隔板的直桶,或者是一个包围着例如,真空罐或低温管道的内容器且带有径向的或平面的(例如水平的)隔板的圆环形盒。
这种容器可以是刚性,半刚性或挠性的盒子,由不含水的材料,最好是金属,玻璃,陶瓷或它们的复合物制成。它也可是圆环状的,其横截面可采用不同的形状即圆形,方形,矩形,三角形,椭圆形,卵形,瓣叶形及类似形状。
下面的例子是为了说明而提供的,它不以任何方式限制本发明的应用范围。
例1
这个例子的目的是为了说明如图1所示的真空罐的性能,它具有一个不是利用本发明的方法制造的真空套。
所述真空套的容量为36升,含有500克的多层绝缘材料,这种绝缘材料由聚烯烃带和涂铝的聚酯带交替重叠构成(商业上称为MYLAR(聚酯薄膜)带),真空套与外面的回转型和涡轮分子型真空泵相连,可维持泵送5小时。随后,真空罐被隔离,压力的增加随着时间的变化开始被记录下来。
这些试验的结果如图2的线1所示。而线2则表示仅仅由于空气通过真空罐中的泄漏处而进入套中所引起的压力增加,约为6×10-7帕·米3/秒的数量级,此线是根据质谱仪测量结果画出的。被试验的装置相当好地代表了一般所采用的实际装置,然而,为了进行加速试验,创造了一个数值至少为在这种运行情况下容许的值的5000倍(通常约为10-10帕·米3/秒的数量级)的上述漏气处。这样,有可能在短时间内,再现持续长时间泄漏的效应。线1与线2的差别是由于内部绝缘材料所释放出的气体,主要是水造成的。
例2
重复例1的试验,但根据欧洲专利申请No.92830186,在真空套内,在相应于干燥剂10和吸气剂11的区域内,分别放入10克小颗粒(小球丸)状的BaO和10克BaLi4合金,这些小颗粒放在如欧洲专利申请No.92830185公布的热伸缩容器(器皿)中。
真空套与外面的泵相连,并接受10分钟的短期泵吸。然后,关闭阀7使系统与泵隔开。在这种条件下,需要有24小时的吸气时间,接着打开阀7进行第二阶段(重新泵吸系统),同时通过安放在外部与吸气剂的内部位置相对应的地方上的加热装置激活吸气剂至120℃,为此目的通常使用热空气枪。活化时间为25分钟,此后系统断开,开始记录压力随时间的变化。这些试验的结果示于图2的线3。
比较图2的线1和线3可以看出,采用本发明的方法可以大大降低致冷装置密封后的压力增加量。使用质谱仪进行的一些分析试验表明,综合使用两种材料(干燥剂与吸气剂),不仅可以定量地吸收绝缘材料释出的水,而且可以贴补装置的泄漏处。另外,还应该意识到,试验是在加速条件下进行的,即在比实际情况更苛刻的条件下进行的,如象在大气的压力下一样。因此,持续360小时(15天)的加速试验相当于实际工作至少20年。
应当理解,熟悉本技术的人员对于在上述工作条件下所进行的任意增添和/或改变不会偏离本发明的领域和精神。
Claims (16)
1、一种用于绝热套(5),特别是真空瓶或另一种致冷装置(1)的绝热套(5)的抽真空和生产准备的改进方法,致冷装置具有内壁(2)和外壁(4),并在所述壁面之间有一内层空间,它完全地或部分地填入绝缘材料(9),所述内层空间还包含有吸湿剂(10)和吸气剂(11),其特征在于所述吸湿剂(10)是化学干燥剂。
2、根据权利要求1的方法,其特征在于所述化学干燥剂在室温下的H2O蒸汽压力低于1帕(Pa),并且最好选用氧化钡,氧化锶,氧化磷及它们的混合物。
3、根据权利要求1的方法,其特征在于下列步骤:
A.套(5)的内层空间首先用真空泵抽真空至压力低于100帕(Pa);
B.所述内层空间同时受到所述化学干燥剂(10)的作用,而吸气剂(11)则保持在非活化状态;
C.所述内层空间再用真空泵抽真空至压力低于5帕(Pa);
D.激活所述的吸气剂(11);
E.通过切断所述泵与外套内层空间之间的连接而使外套与泵隔开。
4、根据权利要求3的方法,其特征在于在步骤B进行过程中,根据步骤A的泵吸作用停止。
5、根据权利要求3的方法,其特征在于在步骤A与B的过程中,所述真空罐或另一个致冷装置的内壁(2)保持是热的,温度不高于150℃,最好为120℃,这样可促使水从绝缘材料(9)中释出。
6、根据权利要求3,4,5中任一个所述的方法,其特征在于步骤B持续不超过48小时,最好为2至48小时。
7、根据权利要求3的方法,其特征在于所述化学干燥剂(10)和所述吸气剂(11)放于分开的位置,且贴到所述真空罐或其他致冷装置的外壁(4)上。
8、根据权利要求7的方法,其特征在于所述化学干燥剂(10)和所述吸气剂(11)放在容器(12)中,容器(12)用多孔隔板(13)分割为内区(14)和外区(15),其中
-内区(14)含有所述吸气剂(11);
-外区(15)与含有绝缘材料(9)的内层空间相通,并含有所述化学干燥剂(10),它可防止水蒸汽穿过隔板(13)而流向所述吸气剂(11)。
9、根据权利要求8的方法,其特征在于所述容器(12)为一垂直桶,它带有一个开口和一平面隔板(13),开口位于其最上部。
10、根据权利要求8的方法,其特征在于所述容器(12)为一圆环状盒,它具有径向或平面隔板(13)。
11、根据权利要求9或10的方法,其特征在于所述隔板(13)为水平的。
12、根据权利要求8的方法,其特征在于所述容器(12)为一刚性,半刚性或柔性的盒。
13、根据权利要求8的方法,其特征在于所述容器(12)的横截面形状可以是圆形,方形,矩形,三角形,椭圆形,卵形,瓣叶形及类似形状。
14、根据权利要求8的方法,其特征在于所述容器(12)是由完全不含水的材料制成,并选用金属,玻璃,陶瓷及它们的复合物。
15、根据上述权利要求中任一项的方法,其特征在于所述吸气剂(11)选用含有钡和锂的合金。
16、根据权利要求14的方法,其特征在于所述吸气剂(11)为一种原始分子式为BaLi4的合金。
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ITMI921416A IT1258958B (it) | 1992-06-08 | 1992-06-08 | Processo perfezionato per la realizzazione di intercapedini termicamente isolanti mediante vuoto e materiali coibenti |
ITMI92A001416 | 1992-06-08 |
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KR (1) | KR100253841B1 (zh) |
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WO (1) | WO1993025842A1 (zh) |
Cited By (5)
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CN102205228A (zh) * | 2010-05-27 | 2011-10-05 | 福建赛特新材股份有限公司 | 用于维持中低真空环境的复合吸气剂及其制备方法 |
CN102913749A (zh) * | 2012-10-23 | 2013-02-06 | 西安轨道交通装备有限责任公司 | 大容积低温绝热容器用抽真空系统及方法 |
CN103249644A (zh) * | 2010-10-27 | 2013-08-14 | 高级技术材料公司 | 用于去除杂质的基于衬里的组件 |
CN104685285A (zh) * | 2012-05-11 | 2015-06-03 | 欧瑞康先进科技股份公司 | 用于真空隔绝的管路的适配器 |
CN113226913A (zh) * | 2018-12-28 | 2021-08-06 | 川崎重工业株式会社 | 船舶 |
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IT1264692B1 (it) * | 1993-07-08 | 1996-10-04 | Getters Spa | Combinazione di getter adatta per camicie isolanti sotto vuoto reversibile |
JPH08159377A (ja) * | 1994-12-02 | 1996-06-21 | Matsushita Refrig Co Ltd | 真空断熱体 |
US7854236B2 (en) * | 2007-06-19 | 2010-12-21 | Praxair Technology, Inc. | Vacuum insulated piping assembly method |
KR101068459B1 (ko) | 2010-07-29 | 2011-09-28 | 주식회사엑스엘 | 진공단열패널 |
US10295447B2 (en) | 2017-07-10 | 2019-05-21 | Cem Corporation | Rapid energized dispersive solid phase extraction (SPE) for analytical analysis |
US10330573B2 (en) | 2017-07-10 | 2019-06-25 | Cem Corporation | Rapid sample preparation for analytical analysis using dispersive energized extraction |
US10241014B2 (en) | 2017-07-10 | 2019-03-26 | Cem Corporation | Instrument for analytical sample preparation |
GB2584443A (en) * | 2019-06-03 | 2020-12-09 | Linde Kryotechnik Ag | Vacuum insulated equipment |
KR102303797B1 (ko) * | 2020-03-23 | 2021-09-17 | 한국과학기술원 | 증발량 조절이 가능한 액체 수소 저장 장치 |
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US3114469A (en) * | 1963-02-20 | 1963-12-17 | Union Carbide Corp | Means for improving thermal insulation space |
FR1422353A (fr) * | 1964-11-13 | 1965-12-24 | Thomson Houston Comp Francaise | Enceinte calorifugée à température interne sensiblement constante |
NL7412693A (nl) * | 1974-09-26 | 1976-03-30 | Philips Nv | Getterhouder en elektrische ontladingsbuis voorzien van een dergelijke houder. |
DE2657904A1 (de) * | 1975-12-30 | 1977-07-14 | Osaka Oxygen Ind | Thermosbehaelter fuer verfluessigte gase und getterlegierung dafuer |
DE2902623A1 (de) * | 1979-01-24 | 1980-07-31 | Messer Griesheim Gmbh | Verfahren und getteranordnung zur aufrechterhaltung eines vakuums |
US4997124A (en) * | 1988-04-20 | 1991-03-05 | Zojirushi Corporation | Vacuum-insulated, double-walled metal structure and method for its production |
-
1992
- 1992-06-08 IT ITMI921416A patent/IT1258958B/it active IP Right Grant
- 1992-11-09 WO PCT/IT1992/000141 patent/WO1993025842A1/en active Application Filing
- 1992-11-30 CN CN92113646A patent/CN1029154C/zh not_active Expired - Fee Related
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102205228A (zh) * | 2010-05-27 | 2011-10-05 | 福建赛特新材股份有限公司 | 用于维持中低真空环境的复合吸气剂及其制备方法 |
CN102205228B (zh) * | 2010-05-27 | 2013-05-08 | 福建赛特新材股份有限公司 | 用于维持中低真空环境的复合吸气剂及其制备方法 |
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CN103249644B (zh) * | 2010-10-27 | 2016-05-18 | 高级技术材料公司 | 用于去除杂质的基于衬里的组件 |
CN104685285A (zh) * | 2012-05-11 | 2015-06-03 | 欧瑞康先进科技股份公司 | 用于真空隔绝的管路的适配器 |
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CN113226913A (zh) * | 2018-12-28 | 2021-08-06 | 川崎重工业株式会社 | 船舶 |
Also Published As
Publication number | Publication date |
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WO1993025842A1 (en) | 1993-12-23 |
IT1258958B (it) | 1996-03-11 |
ITMI921416A0 (it) | 1992-06-08 |
KR950701056A (ko) | 1995-02-20 |
CN1029154C (zh) | 1995-06-28 |
ITMI921416A1 (it) | 1993-12-08 |
KR100253841B1 (ko) | 2000-04-15 |
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