石油炼制与化工 ›› 2016, Vol. 47 ›› Issue (4): 23-29.

• 基础研究 • 上一篇    下一篇

焙烧温度对无黏结剂5A小球吸附剂性能的影响

王红超,王辉国,刘宇斯,杨彦强   

  1. 中国石化石油化工科学研究院
  • 收稿日期:2015-09-21 修回日期:2015-11-03 出版日期:2016-04-12 发布日期:2016-04-19
  • 通讯作者: 王红超 E-mail:wanghc.ripp@sinopec.com

EFFECT OF CALCINATION TEMPERATURE ON METHANOL ADSORPTION PERFORMANCE OF BINDERLESS 5A SPHERICAL ADSORBENT

  • Received:2015-09-21 Revised:2015-11-03 Online:2016-04-12 Published:2016-04-19

摘要:

对由高岭土和NaA分子筛成型得到的NaA小球进行焙烧,将部分焙烧后小球进行碱处理和Ca2+交换,采用TG-DTA、XRD、27Al-NMR、甲醇吸附、氮气物理吸附等方法对样品进行表征和评价, 考察焙烧温度对其物性和吸附性能的影响。结果表明:在 500~700 ℃焙烧能够使高岭土结构坍塌成为偏高岭土,但不会破坏NaA分子筛结构,经碱处理后偏高岭土几乎全部转变为NaA分子筛,其中经700 ℃焙烧后碱处理的小球吸附量最高;在750℃焙烧可使NaA分子筛骨架结构发生变化,几乎丧失对甲醇的吸附能力,但经碱处理后不仅偏高岭土转变为NaA分子筛,而且小球内原有的分子筛结构得到了修复,使得小球的甲醇吸附量高于NaA分子筛原粉;焙烧温度超过800 ℃时, NaA分子筛会转变成更加稳定的三斜霞石或霞石;在750 ℃焙烧再经碱处理和Ca2+交换制备的5A小球的灼基堆密度和抗压碎强度明显优于700 ℃以下焙烧制备的5A小球,其原因是较高的温度导致小球内微粒的结合更紧密。

关键词: NaA小球, NaA分子筛, 5A小球吸附剂, 焙烧温度, 碱处理

Abstract:

The NaApellets composed of kaolin and NaA molecular sieve were calcinated,and the small pellets were successivelytreated with alkali solutionand exchanged with Ca2+solution. Samples were characterized and evaluated by TG-DTA, XRD, 27Al-NMR, methanol adsorption, nitrogen physical adsorption and pulse test. The results showedthat kaolininNaApelletswas changedintometakaolinduring calcinations at 500-700 ℃, and the latter was converted to NaAmolecular sieve after alklitreatment.When calcinated at 750 ℃,NaA molecular sieve in pellets was changed in structure and lost adsorption capacity of methol, however,afteralkali treatment, not only kaolin in pellets was converted to NaA molecular sieve, but alsothe destroyedNaA molecular sieve was repairedandhad higher adsorption capacity than uncalcinedNaA. When calcination temperature was above 800 ℃, NaAwas transformed into more stable carnegeiteand nepheline. Physical analysis and mercury intrusion showed that, NaApelletscalcinatedat750 ℃ had larger apparent bulk density and crush strength compared to thatcalcinatedbelow 700 ℃。This was because particlesin pelletsbindsmore tightly during higher temperature.

Key words: NaA pellet, NaA molecular sieve, 5A pellet adsorbent, calcination temperature, alkali treatment