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A kind of amine functionalized adsorbent and preparation method thereof

An amine functionalization and adsorbent technology, applied in the field of molecular sieves, can solve problems such as poor adsorption and removal, achieve high-efficiency adsorption, avoid loss, and increase loading.

Active Publication Date: 2018-09-11
ELECTRIC POWER RES INST OF GUANGDONG POWER GRID
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the selective adsorption and removal of water by this molecular sieve is poor

Method used

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  • A kind of amine functionalized adsorbent and preparation method thereof
  • A kind of amine functionalized adsorbent and preparation method thereof

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preparation example Construction

[0045] The present invention also provides a preparation method of amine functionalized adsorbent, comprising the following steps:

[0046] A) mixing an alkylamine template, tetraethylorthosilicate and a doping modifier in a solvent for doping modification to obtain a doping-modified HMS molecular sieve;

[0047] The doping modifier includes one or more of Zr precursors, Ti precursors and Al precursors;

[0048] B) using an organic amine modifier to modify the doped modified HMS molecular sieve to obtain an amine functionalized adsorbent;

[0049] The organic amine modifier includes one or more of tetraethylenepentamine, pentaethylenehexamine, polyethylenepolyamine, and polyethyleneimine.

[0050] In the present invention, the alkylamine template is preferably added into the solvent, stirred evenly, and then tetraethyl orthosilicate (TEOS) and the doping modifier are added, and the doping modification is carried out under stirring conditions to obtain the doped Modified HMS ...

Embodiment 1

[0062] The doping modification of HMS molecular sieve can be realized by replacing a certain proportion of tetraethyl orthosilicate with a doping modifier. press n 异丙醇铝 :n 正硅酸乙酯 :n 十二烷基胺 :n CH3CH2OH :n H2O =0.03::0.97:0.27:6.50:36.00 molar ratio Add dodecylamine templating agent into 400ml water-ethanol solvent, stir well at 40°C, then slowly add tetraethyl orthosilicate (TEOS) and iso Aluminum propoxide, continued to stir for 24 hours, and vacuum-dried to obtain an Al-doped modified HMS molecular sieve (3Al-DDA-HMS).

[0063] Dissolve 1g polyethyleneimine (PEI) in methanol solution, stir at room temperature for 60min, add 4g of 3Al-DDA-HMS, stir for another 6h, and vacuum dry to obtain 20PEI / 3Al-DDA-HMS adsorbent.

[0064] In the experiment, the adsorption capacity of 20PEI / 3Al-DDA-HMS was tested according to the national standard GB 6287-86 molecular sieve static water adsorption determination method. First, vacuum-dry the adsorbent in an oven at 105°C for 24 hours, th...

Embodiment 2

[0067] press n 氯氧化锆 :n 正硅酸乙酯 :n 十二烷基胺 :n CH3CH2OH :n H2O =0.05::0.95:0.27:7:36.00 molar ratio Add dodecylamine (DDA) into a mixed solution of 300ml water and ethanol, stir well at 50°C, slowly add tetraethyl orthosilicate (TEOS) and Zirconium oxychloride, continue stirring for 12 hours, and vacuum-dry to obtain doped modified HMS molecular sieve (5Zr-DDA-HMS). Finally, dissolve 1.7143g of pentaethylenehexamine (PEHA) in methanol solution, stir at room temperature for 30min, add 4g of 5Zr-DDA-HMS, stir for another 2h, and vacuum dry to obtain 30PEHA / 5Zr-DDA-HMS.

[0068] In the experiment, the static water absorption capacity of 30PEHA / 5Zr-DDA-HMS is 15%, which is 12% higher than that of the 5Zr-DDA-HMS sample modified without amine loading; the decomposition temperature of 30PEHA / 5Zr-DDA-HMS in the experiment is 187°C, which is 82°C higher than that of the 30PEHA / DDA-HMS sample modified without zirconium doping.

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Abstract

The invention provides an amino-functionalized adsorption agent and a preparation method thereof.The amino-functionalized adsorption agent is obtained in the mode that a doped modified HMS molecular sieve is modified through an organic amino modification agent.The doped modified HMS molecular sieve is obtained by performing doping modification on an HMS molecular sieve through a doping modification agent.The doping modification agent is selected from one or more of a Zr precursor, a Ti precursor and a Al precursor.The HMS molecular sieve is subjected to doping modification through the doping modification agent firstly, certain acid sites are introduced to the pipe wall of the molecular sieve, then organic amino modification is conducted, accordingly organic amino can be loaded and polymerized on the HMS molecular sieve more effectively, the loading amount is increased, and efficient adsorption of water molecules is achieved.Besides, the amino-functionalized adsorption agent is good in stability, and the shell protection effect of a mesoporous channel can effectively avoid the problem that active sites lose in the long-time adsorption process of an adsorption agent.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, in particular to an amine functionalized adsorbent and a preparation method thereof. Background technique [0002] Given SF 6 High chemical stability and good insulation performance, SF has been widely used in the world 6 As an insulating medium for various electrical equipment. But SF 6 In the manufacturing process, there are inevitably traces of low-fluoride and moisture; the action of high-voltage arcs in the operation of equipment makes SF 6 Also decomposes a small amount of low fluoride, such as: SF 4 、SOF 2 , SO 2 f 2 , S 2 f 10 O et al. And when there is a trace of water, these low fluorides gradually decompose into HF, SO 2 、H 2 SO 4 Such strong corrosive properties are not only harmful to the human body, but also seriously corrode electrical equipment. At present, both at home and abroad, the method of placing adsorbents in electrical equipment to remove harmful im...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/30B01J20/18B01J20/26
CPCB01J20/18B01J20/186B01J20/261B01J2220/4806B01J2220/4812B01J2220/68
Inventor 李丽唐念刘洁樊小鹏黎晓淀黄成吉刘嘉文
Owner ELECTRIC POWER RES INST OF GUANGDONG POWER GRID
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