CN106466596B - It is a kind of using Zylon fiber coats as the preparation method of the whole needle type extraction device of medium - Google Patents
It is a kind of using Zylon fiber coats as the preparation method of the whole needle type extraction device of medium Download PDFInfo
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- CN106466596B CN106466596B CN201510512001.9A CN201510512001A CN106466596B CN 106466596 B CN106466596 B CN 106466596B CN 201510512001 A CN201510512001 A CN 201510512001A CN 106466596 B CN106466596 B CN 106466596B
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Abstract
The invention belongs to organic composite materials and technical field, the preparation method of whole needle type extraction device is filled more particularly to a kind of fiber, specifically using Zylon fibers as filler, it is coated using benzoic acid as template molecule on its surface, using 4-vinylpridine as function monomer, the molecularly imprinted polymer coating that is prepared as crosslinking agent using ethylene glycol dimethacrylate.Since the specific surface area of fiber is very big, the amount of polymer coating will increase and more uniformly, to increase extraction efficiency, it is ensured that the accumulation ability of extraction equipment.
Description
Technical field
The invention belongs to organic composite materials and technical field, and in particular to a kind of whole pin type extraction of fiber coat filling
The preparation method of device, the extraction equipment of research and development can be used for the selective enrichment of Environmental Trace gas component.
Background technology
Pin type abstraction technique mainly carries out pre-treatment, which can be with molecule as a kind of new technique to complex sample
Engram technology is combined, and has many advantages, such as high selectivity, and stability is good and adsorption capacity is strong, can be combined with gas-chromatography for waving
The extraction and detection of hair property or half volatile trace components.
However, grow up in the recent period can with molecular engram integral column extraction equipment associated with gas-chromatography instrument, be
Whole fabricated in situ in stainless pin, along with device needs are matched with gas chromatographic sample introduction mouth so that generate polymer
Amount is difficult to control, and permeability is poor, and polymer is easy to fall off out of needle to damage instrument during thermal desorption.
The present invention prepares molecularly imprinted polymer coating in the good Zylon fiber surfaces of thermal stability, due to the ratio of fiber
Surface is big, it is ensured that the extraction efficiency and accumulation ability of coating media.In addition, not being coupled between fibre bundle, in extraction process
In improve the permeability of extraction equipment, reduce back pressure, while also improving the mechanical strength of extraction equipment, extend device
Service life.
Invention content
The object of the present invention is to provide a kind of using Zylon fiber coats as the preparation side of the whole needle type extraction device of medium
Method.Specifically invention content is：
(1) fiber, capillary glass tube acetone, washes of absolute alcohol is clean, it is dried up at ambient temperature with nitrogen standby
With；
(2) the true fibre of certain amount is longitudinally therethrough in capillary glass tube；
(3) by template molecule benzoic acid, function monomer 4-vinylpridine（4-VP）, crosslinking agent ethylene glycol dimethyl propylene
Acid esters（EDMA）, initiator azodiisobutyronitrile（AIBN）, solvent lauryl alcohol and toluene are put into sample bottle, are surpassed by a certain percentage
After sound dissolves mixing, nitrogen blows down oxygen, and pre-polymer solution is made；
(4) by pre-polymer solution implantation glass capillary, then put into small test tube and sealed, put into baking oven and react
A few hours；
(5) the reaction was complete takes out fiber, is placed on eluent（Sodium hydroxide/absolute ethyl alcohol volume ratio is 1/4）Middle elution mould
Plate molecule, cleaning are washed till neutrality with absolute ethyl alcohol again completely, and nitrogen drying is made the fiber with molecular engram coating and is situated between
Matter；
There to be the fiber of polymer coating to penetrate in stainless pin and carries out aging to get to fiber coat molecular engram needle
Formula extraction equipment.
Description of the drawings
Fig. 1 is the vapor detection figure using fiber coat molecular engram needle type extraction device benzene-series-enricmolecularly.
Specific implementation mode
Polymer prepares embodiment：
By benzoic acid, 4-vinylpridine, EDMA is according to 1:3:30 ratio, toluene:Lauryl alcohol is according to 1:12.5 ratio
Example 5~10min of ultrasonic dissolution mixing in sample bottle, nitrogen blow down oxygen, are injected into pre-polymer solution with syringe and are installed with fiber
Capillary glass tube in, then capillary is fitted into test tube sealing and puts in baking oven polymerisation 22h at 60 DEG C into, to the end of reaction
The template molecule on fiber sodium hydroxide/ethanol solution eluting fibers surface is taken out afterwards, then with absolute ethyl alcohol by fiber
It is washed till neutrality, then fiber is penetrated in chromatography column feed materials mouth aging in stainless pin, for use.
Polymer application example：
The gaseous sample of 5 μ g/L of fiber coat molecular engram needle type extraction device pair obtained in aforementioned manners（Benzene, first
Benzene, ethylbenzene, ortho-xylene）It carries out repeatedly sampling and in gas chromatographic sample introduction mouth desorption under high temperature, completes gas-chromatography to gas sample
The separation detection of product, chromatogram are as shown in Fig. 1.
Claims (1)
1. a kind of preparation method of fiber coat needle type extraction device for benzene-series-enricmolecularly is using benzoic acid as template point
Son, 4-vinylpridine are function monomer, and ethylene glycol dimethacrylate is crosslinking agent, and lauryl alcohol and toluene are solvent, even
Nitrogen bis-isobutyronitrile is initiator, the synthetic polymer coating on true fibre, then fiber treatment is penetrated stainless pin
Needle type extraction device is inside made, it is characterised in that：
(1) stainless pin needed for testing is standard 21G, length 5cm, 300 DEG C of high temperature resistant or more；
(2) fiber needed for testing is Zylon HM fibers, and it is 0.5mm that the Zylon fibers of 350~400 beams or so, which are penetrated internal diameter,
Capillary glass tube in；
(3) molar ratio of sample is benzoic acid in pre-polymer solution:4-vinylpridine:Ethylene glycol dimethacrylate=1:
3:30；
(4) coating preparation process needs successive reaction 20h~for 24 hours in an oven, oven temperature to control at 50 DEG C~60 DEG C；
(5) eluent used in experiment is 0.2mol/L sodium hydroxides/absolute ethyl alcohol, volume ratio 1:4.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510512001.9A CN106466596B (en) | 2015-08-20 | 2015-08-20 | It is a kind of using Zylon fiber coats as the preparation method of the whole needle type extraction device of medium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510512001.9A CN106466596B (en) | 2015-08-20 | 2015-08-20 | It is a kind of using Zylon fiber coats as the preparation method of the whole needle type extraction device of medium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106466596A CN106466596A (en) | 2017-03-01 |
| CN106466596B true CN106466596B (en) | 2018-10-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510512001.9A Active CN106466596B (en) | 2015-08-20 | 2015-08-20 | It is a kind of using Zylon fiber coats as the preparation method of the whole needle type extraction device of medium |
Country Status (1)
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107860853A (en) * | 2017-12-15 | 2018-03-30 | 吉林化工学院 | A kind of needle type extraction device and its application method for concentrating volatile benzene homologues |
| CN112063005B (en) * | 2020-09-08 | 2022-12-06 | 吉林化工学院 | Preparation method of molecular imprinting integral needle type extraction device for enriching polychlorinated biphenyl |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240066A (en) * | 2013-04-28 | 2013-08-14 | 西安交通大学 | Preparation method of molecularly imprinted polymer coating solid-phase microextraction fiber |
| CN103509155A (en) * | 2013-07-19 | 2014-01-15 | 吉林化工学院 | Method for improving permeability and mechanical strength of molecular imprinting integral needle-type extraction device |
| CN103533998A (en) * | 2011-03-08 | 2014-01-22 | 纳瑙佩颇公司 | High-performance fibrous products |
-
2015
- 2015-08-20 CN CN201510512001.9A patent/CN106466596B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103533998A (en) * | 2011-03-08 | 2014-01-22 | 纳瑙佩颇公司 | High-performance fibrous products |
| CN103240066A (en) * | 2013-04-28 | 2013-08-14 | 西安交通大学 | Preparation method of molecularly imprinted polymer coating solid-phase microextraction fiber |
| CN103509155A (en) * | 2013-07-19 | 2014-01-15 | 吉林化工学院 | Method for improving permeability and mechanical strength of molecular imprinting integral needle-type extraction device |
Non-Patent Citations (1)
| Title |
|---|
| 纤维填充整体针式萃取装置的制备及其性能研究;杨巧玲等;《分析化学》;20140430;第42卷(第4期);第507-512页 * |
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