CN112778012A - 一种高温熔盐管道的制备方法 - Google Patents
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Abstract
本发明涉及一种高温熔盐管道的制备方法,其包括步骤:S1,通过石墨加工形成内衬;S2,采用化学气相沉积的方法在内衬的外表面上形成均匀致密的防渗层;S3,将浸渍过酚醛树脂的碳纤维作为碳纤维增强材料均匀缠绕到防渗层上得到第一制品;S4,将第一制品进行固化处理得到第二制品;S5,将第二制品进行碳化和石墨化处理得到高温熔盐管道。根据本发明的高温熔盐管道的制备方法,采用碳纤维对石墨管道进行增强,并采用防渗夹层使管道拥有良好的防渗效果。
Description
技术领域
本发明涉及高温熔盐储能领域,更具体地涉及一种高温熔盐管道的制备方法。
背景技术
熔盐是一种良好的热载体,近年来在能源及化工领域开始获得广泛应用,例如熔盐堆、熔盐储能以及熔盐热处理等。由于熔盐具有较高的熔点、较强的腐蚀性等,采用一般的合金作为管道有许多的困难需要克服,特别是将熔盐运用在超高温领域。
炭材料以其优异的耐热性、低热膨胀系数、优异的抗热冲击性等优点广泛应用于化工行业,将炭材料的优异性能应用在超高温熔盐领域是一种必然的趋势。但是以石墨为代表的炭材料较脆,采用常规的炭材料管道给项目设计及安全带来一定挑战。因此,为高温熔盐设计并研发满足使用要求的高温熔盐传输的管道成为高温熔盐发展亟需解决的技术问题。
发明内容
为了解决现有技术中的高温熔盐对管道具有较高要求的问题,本发明提供一种高温熔盐管道的制备方法。
根据本发明的高温熔盐管道的制备方法,其包括步骤:S1,通过石墨加工形成内衬;S2,采用化学气相沉积的方法在内衬的外表面上形成均匀致密的防渗层;S3,将浸渍过酚醛树脂的碳纤维作为碳纤维增强材料均匀缠绕到防渗层上得到第一制品;S4,将第一制品进行固化处理得到第二制品;S5,将第二制品进行碳化和石墨化处理得到高温熔盐管道。
根据本发明的高温熔盐管道的制备方法,以石墨作为内衬并在其外表面制作防渗层,碳纤维缠绕防渗层形成石墨和碳纤维缠绕复合材料,其力学和化学性能沿管道轴向均一、阻挡熔盐浸渗、控制气体泄露、强度和韧性满足高温熔盐结构安全性。
优选地,在所述步骤S1中,石墨为密度在1.7-2.2g/cm3的高纯石墨材料。在优选的实施例中,石墨为密度在1.8-2.0g/cm3的高纯石墨材料。
优选地,在所述步骤S2中,防渗层为碳层或碳化硅层。其通过化学气相沉积的方法结合在石墨内衬上。在优选的实施例中,
优选地,在所述步骤S2中,防渗层的厚度为2-3mm。
优选地,在所述步骤S3中,碳纤维增强材料根据最终产品使用温度和熔盐环境的需求确定规格。
优选地,在所述步骤S3中,碳纤维为T700级碳纤维或T1000级碳纤维。
优选地,在所述步骤S3中,碳纤维增强材料通过纤维缠绕机张力控制系统缠绕到防渗层上。
优选地,在所述步骤S3中,纤维缠绕机张力控制系统以3-10kg的张力在防渗层上均匀缠绕碳纤维增强材料。
优选地,在所述步骤S3中,缠绕温度为25-40℃,缠绕角度为0°-90°,缠绕层的厚度为5-6mm。
优选地,在所述步骤S3中,酚醛树脂为热固性酚醛树脂。
优选地,在所述步骤S4中,在40-50℃下保温2h,然后再缓慢升温至60-70℃保温2h,进行固化。更优选地,为保证制品性能,固化过程不宜少于5h。
优选地,在所述步骤S5中,第二制品经过反复的酚醛树脂浸渍和碳化进行增密直至缠绕层密度为1.6~1.9g/cm3,最后石墨化成型。具体地,首先将第二制品在保护气氛(例如氮气)下以一定的速率(例如0.05-0.5℃/Min)升温至850-1300℃进行碳化,然后把碳化处理的制品继续放入高压反应釜(例如在压力2-4MPa下)继续酚醛树脂浸渍,循环增密6-8次,最后将经过多次增密处理的制品在保护气氛下升温至2000-3000℃进行石墨化处理,即得高温熔盐管道。
根据本发明的高温熔盐管道的制备方法,采用碳纤维对石墨管道进行增强,并采用防渗夹层使管道拥有良好的防渗效果。本发明提供的工艺过程成熟、生产的熔盐管件的外形、长度设计不受限制。采用本发明制备的管道有耐高温、耐熔盐腐蚀、耐高压和性能均一等特点,是熔盐管道的理想材料。总之,根据本发明的高温熔盐管道,质量轻、空隙率低、纤维含量高、韧性高、耐中子辐照、熔盐浸渗性好,特别适合应用于高温熔盐。
具体实施方式
下面给出本发明的较佳实施例,并予以详细描述。
实施例1
根据控制棒套管的外形,加工一根长3000mm,内径60mm,外径70mm,底部为U形,上部开口的石墨芯材。
将密度为1.80g/cm3的高纯石墨芯材作为基体,然后以三氯甲基硅烷(MTS)为先驱体原料,氢气为载气、氩气为稀释气在950-1300℃范围内通过化学气相沉积一层2mm的碳化硅防渗层。
使用T700级碳纤维作为增强体,通过数控纤维缠绕机对浸渍过酚醛树脂的碳纤维对生成碳化硅涂层的芯材进行均匀缠绕,缠绕温度范围25-40℃、张力3-5kg、角度0°-25°,缠绕厚度5-6mm,所用的树脂为热固性酚醛树脂。
将上面缠绕成型的制品放入固化炉中进行固化处理,首先在40-50℃保温2h,然后再缓慢升温至60-70℃保温2h,为保证制品性能,固化过程不宜少于5h。
先将固化处理的制品在氮气保护下以0.05-0.5℃/Min速率升温至850-1300℃进行碳化,然后把碳化处理的制品继续放入高压反应釜在压力2-4MPa继续浸渍,增密6-8次后将制品在保护气氛下升温至2000-3000℃石墨化处理,直到缠绕层密度为1.6~1.9g/cm3。
本实施例的熔盐堆控制棒套管的质量轻、空隙率低、纤维含量高、韧性好、耐中子辐照、熔盐浸渗性好、性能均一等优点且能耐40-60MPa的压力。
实施例2
通过密度为2.0g/cm3的高纯石墨材料制作一根外径100mm,内径80mm的石墨管。
将石墨管放入沉积炉,用甲烷作为碳源进行热解碳防渗层的生成。在1000-1500℃温度范围、300-800ml/min甲烷流量、压力为6-12KPa、经过4-6h生成2-3mm的热解碳涂层。
选用T1000级碳纤维作为增强体,通过数控纤维缠绕机在制备好热解碳涂层的石墨表面进行碳纤维缠绕,缠绕温度范围25-40℃、张力5-10kg、角度85°-90°、缠绕厚度5-6mm。
将缠绕好的制品放入高压反应釜在压力2-5MPa时间6-10h浸渍酚醛树脂,将浸渍完成的样品在压力1-2MPa、温度120-180℃、时间5-6h完成固化。
先将固化处理的制品在氮气保护下以0.05-0.5℃/Min速率升温至850-1300℃进行碳化,然后把碳化处理的制品继续放入
高压反应釜在压力2-4MPa继续浸渍,增密6-8次后将制品在保护气氛下升温至2000-3000℃石墨化处理,直到缠绕层密度1.6~1.9g/cm3。
本实施例的高温熔盐管质量轻、空隙率低、纤维含量高、韧性好、熔盐浸渗性好、性能均一等优点且能耐80MPa以上压力。
以上所述的,仅为本发明的较佳实施例,并非用以限定本发明的范围,本发明的上述实施例还可以做出各种变化。即凡是依据本发明申请的权利要求书及说明书内容所作的简单、等效变化与修饰,皆落入本发明专利的权利要求保护范围。本发明未详尽描述的均为常规技术内容。
Claims (10)
1.一种高温熔盐管道的制备方法,其特征在于,包括步骤:
S1,通过石墨加工形成内衬;
S2,采用化学气相沉积的方法在内衬的外表面上形成均匀致密的防渗层;
S3,将浸渍过酚醛树脂的碳纤维作为碳纤维增强材料均匀缠绕到防渗层上得到第一制品;
S4,将第一制品进行固化处理得到第二制品;
S5,将第二制品进行碳化和石墨化处理得到高温熔盐管道。
2.根据权利要求1所述的制备方法,其特征在于,石墨为密度在1.7-2.2g/cm3的高纯石墨材料。
3.根据权利要求1所述的制备方法,其特征在于,防渗层为碳层或碳化硅层。
4.根据权利要求1所述的制备方法,其特征在于,防渗层的厚度为2-3mm。
5.根据权利要求1所述的制备方法,其特征在于,碳纤维为T700级碳纤维或T1000级碳纤维。
6.根据权利要求1所述的制备方法,其特征在于,碳纤维增强材料通过纤维缠绕机张力控制系统缠绕到防渗层上。
7.根据权利要求6所述的制备方法,其特征在于,纤维缠绕机张力控制系统以3-10kg的张力在防渗层上均匀缠绕碳纤维增强材料。
8.根据权利要求1所述的制备方法,其特征在于,缠绕温度为25-40℃,缠绕角度为0°-90°,缠绕层的厚度为5-6mm。
9.根据权利要求1所述的制备方法,其特征在于,在所述步骤S4中,在40-50℃下保温2h,然后再缓慢升温至60-70℃保温2h,进行固化。
10.根据权利要求1所述的制备方法,其特征在于,在所述步骤S5中,第二制品经过反复的酚醛树脂浸渍和碳化进行增密直至缠绕层密度为1.6~1.9g/cm3,最后石墨化成型。
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