CN109173981A - A kind of preparation method of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber - Google Patents
A kind of preparation method of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber Download PDFInfo
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- CN109173981A CN109173981A CN201810888611.2A CN201810888611A CN109173981A CN 109173981 A CN109173981 A CN 109173981A CN 201810888611 A CN201810888611 A CN 201810888611A CN 109173981 A CN109173981 A CN 109173981A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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Abstract
The invention discloses a kind of preparation methods of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber, in particular to utilize the silane coupling agent of polyethyleneimine amino-functionalization, generate polyethyleneimine functionalized SiO 2 airsetting gel coating.This new method is characterized by polyethyleneimine and 3- (2, the third oxygen of 3- epoxy) propyl trimethoxy silicane reaction prepares polyethyleneimine functional silane coupling agent, as preparing precursors, it is bonded airsetting gel coating in basalt fibre surface chemistry, has obtained a kind of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber.Solid-phase micro-extraction fibre prepared by the present invention has good mechanical properties, high surface area and pore structure, show excellent extraction ability, using the solid phase microextraction pipe and liquid chromatograph on-line coupling of its preparation, good application potential is shown in terms of quick, the highly sensitive on-line checking of the Trace Pahs In Water in the fields such as environment measuring, food analysis.
Description
Technical field
The present invention relates to prepare a kind of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
Technology.
Background technique
In-tube SPME is always a kind of important class in solid phase microextraction field, coats extraction coating using inner wall
Tubular material target analytes in fluid sample are extracted.In-tube SPME is often carried out with liquid chromatogram instrument
Analysis system is established in line combination, and the result of analysis method depends on the performance of solid phase microextraction pipe.The performance of solid phase microextraction pipe
Such as extraction selectivity, loading capacity, stability can all have a huge impact analysis result, so high-performance extracting tube
Develop the developing direction of always In-tube SPME.It is that coating coating inner wall or adsorbent are filled out according to solid phase microextraction pipe
It fills in pipe, be divided into blank pipe wall painting type and manage interior adsorbent filled-type two major classes, manage interior adsorbent filled-type than blank pipe wall painting type
Extracting tube has bigger loading capacity, smaller dead volume, it can obtain higher detection sensitivity and more accurately divide
Analyse result.Adsorbent filled-type extracting tube is divided into three kinds again: it is fine that absorbent particles fill extracting tube, integral post extracting tube and extraction
Dimension filling extracting tube.Relative to first two extracting tube, extracting fiber, which fills extracting tube, has extracting pressure low, and preparation is more easier
The advantages that, and extracting fiber restricts the performance of In-tube SPME fiber.
Basalt fibre is a kind of fibrous material of micron order diameter environmentally protective, cheap and easy to get, and surface is rich in a large amount of
Silicone hydroxyl is easy to be chemically modified, and is a kind of good extracting fiber basis material.If a kind of extraction ability is excellent
Coating material is chemically bound on basalt fibre surface, a kind of high performance fiber can be obtained, in In-tube SPME
Aspect has good application potential.Titanium dioxide aeroge is the three-dimensional porous material that a kind of surface area is big, absorption property is strong,
Applied to heavy metal absorbent in heat-barrier material, catalyst carrier, water etc..There is also some disadvantages for aerosil, such as
So that it is not had good adsorptive selectivity because adsorption functional group type is single, the easy fragmentation of pure silicon dioxide aeroge, in order to gram
These problems are taken, chemical modification is often carried out to it using organic group and develops high performance functionalized SiO 2 airsetting glue material
Material.Polyethyleneimine is a kind of organic macromolecule for having multiple amidos, with polycyclic aromatic hydrocarbon, anion etc. have it is stronger mutually
Effect can not only significantly improve its mechanical performance, but also can if carrying out functionalization to aerosil using it
Significantly improve its absorption property.It is reacted, will be transferred in its molecule with silane coupling agent by means of the amido of polyethyleneimine intramolecular
Multiple silane coupling agent groups are connect, in favor of its chemical bonding in aerosil preparation reaction.By polyethyleneimine
The silane coupling agent of amino-functionalization is introduced into the preparing in precursors of aerosil, with ethyl orthosilicate by certain ratio
Example is reacted, and polyethyleneimine functionalized SiO 2 aerogel material is prepared.By means of the silicon hydroxyl on basalt fibre surface
Base participates in the preparation reaction of aeroge, in basalt fibre surface in situ synthesis gas gel coat, obtains high performance polyethylene
Imines functionalized SiO 2 airsetting gel coating is bonded basalt fibre, is a kind of micro- with solid phase in the excellent pipe for extracting potentiality
Fiber material.
Summary of the invention
To prepare polyethyleneimine functionalized SiO 2 airsetting gel coating solid phase micro- the purpose of the present invention is to provide a kind of
The technology of extracting fiber.The present invention is based on polyethyleneimine functional silane coupling agent participate in aerosil preparation,
Airsetting gel coating is prepared in basalt fibre surface in situ, fiber filling polyether-ether-ketone (PEEK) pipe of preparation is developed a kind of solid
Phase extraction pipe, preparation step are specific as follows:
(1) preparation of polyethyleneimine functional silane coupling agent
It in the reactor, is in mass ratio 1:5-8 by polyethyleneimine and 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane
It is dissolved in ethyl alcohol, total mass fraction of the two in reaction solution is 40-60%, uses triethylamine as catalyst, is stirred at reflux
Reaction 16-24 hours removes ethyl alcohol and triethylamine, obtains polyethyleneimine functional silane coupling agent;
(2) preparation of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
In the reactor, using ethyl alcohol as solvent, by polyethyleneimine functional silane coupling agent and ethyl orthosilicate according to matter
For amount than being uniformly mixed for 1:2-3, the mass percentage for controlling reactant is 40-60%, and basalt fibre beam is immersed in reaction
It is 1-2 with hydrochloric acid conditioning solution pH in solution, stirs 6-8 hours formation colloidal sol, adding ammonium hydroxide and adjusting pH is 9, increases temperature
To between 60-80 DEG C, 3-5 hours formation gels are stood, are freeze-dried after carrying out solvent displacement with ethyl alcohol, takes out basalt
Fibre bundle obtains polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber.
The present invention is in the preparation step of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
The solid-to-liquid ratio of the basalt fibre beam and reaction solution is 1:20-30 g/mL.
The present invention is in the preparation step of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
The concentration of hydrochloric acid is 1-2 mol/L.
The present invention is in the preparation step of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
The concentration of the ammonium hydroxide is 1-2 mol/L.
The present invention is in the preparation step of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
Prepared polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber.
It is another object of the present invention to by polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
It gets one's things ready and fills out that an internal diameter is 0.75 mm and length is the polyether-ether-ketone pipe of 40 cm, solid phase microextraction pipe is made, with liquid chromatogram
Instrument on-line coupling, the detection applied to organic micro-pollutant polycyclic aromatic hydrocarbon in water sample.
Polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber prepared by the present invention, and by its
Method for In-tube SPME has the advantage that
(1) functionalization of polyethyleneimine makes aerosil not only increase mechanical strength and improves extractibility
Energy.
(2) in aerosil polyethyleneimine molecular skeleton introducing, make extract coating present in water just
Electrically, there is good absorption property for anion and big pi-conjugated molecule.
(3) on-line coupling is able to carry out with liquid chromatograph, trace analysis object is highly sensitive, highly selective in completion water sample
Analysis detection.
Detailed description of the invention
Fig. 1 is the preparation reaction schematic diagram of polyethyleneimine functional silane coupling agent.
Specific embodiment
For a better understanding of the present invention, it is illustrated by example:
Embodiment 1:
(1) preparation of polyethyleneimine functional silane coupling agent
It in the reactor, is in mass ratio that 1:8 is molten by polyethyleneimine and 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane
For solution in ethyl alcohol, total mass fraction of the two in reaction solution is 40%, uses triethylamine as catalyst, is stirred at reflux reaction
24 hours, ethyl alcohol and triethylamine are removed, polyethyleneimine functional silane coupling agent is obtained;
(2) preparation of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
In the reactor, using ethyl alcohol as solvent, by polyethyleneimine functional silane coupling agent and ethyl orthosilicate according to matter
For amount than being uniformly mixed for 1:3, the mass percentage for controlling reactant is 40%, and basalt fibre beam is immersed in reaction solution
In, it is 2 with 1 mol/L hydrochloric acid conditioning solution pH that the solid-to-liquid ratio of basalt fibre beam and reaction solution, which is 1:30 g/mL, stirring 8
Hour forms colloidal sol, and adding 1 mol/L ammonium hydroxide and adjusting pH is 9, increases temperature to 60 DEG C, stands 5 hours formation gels, use second
Alcohol is freeze-dried after carrying out solvent displacement, is taken out basalt fibre beam, is obtained polyethyleneimine functionalized SiO 2 gas
Gel coat solid-phase micro-extraction fibre.
Embodiment 2:
(1) preparation of polyethyleneimine functional silane coupling agent
It in the reactor, is in mass ratio that 1:5 is molten by polyethyleneimine and 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane
For solution in ethyl alcohol, total mass fraction of the two in reaction solution is 60%, uses triethylamine as catalyst, is stirred at reflux reaction
16 hours, ethyl alcohol and triethylamine are removed, polyethyleneimine functional silane coupling agent is obtained;
(2) preparation of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
In the reactor, using ethyl alcohol as solvent, by polyethyleneimine functional silane coupling agent and ethyl orthosilicate according to matter
For amount than being uniformly mixed for 1:2, the mass percentage for controlling reactant is 60%, and basalt fibre beam is immersed in reaction solution
In, it is 1 with 2 mol/L hydrochloric acid conditioning solution pH that the solid-to-liquid ratio of basalt fibre beam and reaction solution, which is 1:20 g/mL, stirring 6
Hour forms colloidal sol, and adding 2 mol/L ammonium hydroxide and adjusting pH is 9, increases temperature to 80 DEG C, stands 3 hours formation gels, use second
Alcohol is freeze-dried after carrying out solvent displacement, is taken out basalt fibre beam, is obtained polyethyleneimine functionalized SiO 2 gas
Gel coat solid-phase micro-extraction fibre.
Embodiment 3:
(1) preparation of polyethyleneimine functional silane coupling agent
It in the reactor, is in mass ratio that 1:6 is molten by polyethyleneimine and 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane
For solution in ethyl alcohol, total mass fraction of the two in reaction solution is 50%, uses triethylamine as catalyst, is stirred at reflux reaction
20 hours, ethyl alcohol and triethylamine are removed, polyethyleneimine functional silane coupling agent is obtained;
(2) preparation of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
In the reactor, using ethyl alcohol as solvent, by polyethyleneimine functional silane coupling agent and ethyl orthosilicate according to matter
For amount than being uniformly mixed for 1:2.5, the mass percentage for controlling reactant is 50%, and it is molten that basalt fibre beam is immersed in reaction
In liquid, the solid-to-liquid ratio of basalt fibre beam and reaction solution is 1:25 g/mL, is with 1.5 mol/L hydrochloric acid conditioning solution pH
1.5,7 hours formation colloidal sol is stirred, adding 1.5 mol/L ammonium hydroxide and adjusting pH is 9, increases temperature to 70 DEG C, stands 4 hours shapes
It at gel, is freeze-dried after carrying out solvent displacement with ethyl alcohol, takes out basalt fibre beam, obtain polyethyleneimine amino-functionalization
Aerosil coating solid phase micro-extraction fiber.
By the polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction of a branch of 40 cm long and 100 mg weight
Fiber is loaded into 40 cm long and internal diameter is to obtain solid phase microextraction pipe in the PEEK pipe of 0.75 mm.With liquid chromatograph
On-line coupling carries out extraction 15-30 min with the sample flow rate of 1-2 mL/min, and then rotary valve elutes 1-2 min, realizes water
The on-line extraction and analysis detection of 10 kinds of polycyclic aromatic hydrocarbon pollutants of trace level, the range of linearity reach 0.01-20 μ g/ in sample
L, for detection limit down to 0.003 μ g/L, enrichment times are up to 2000 times.
Claims (5)
1. a kind of preparation method of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber, feature exist
In this method has following processing step:
(1) preparation of polyethyleneimine functional silane coupling agent
It in the reactor, is in mass ratio 1:5-8 by polyethyleneimine and 3- (2,3- the third oxygen of epoxy) propyl trimethoxy silicane
It is dissolved in ethyl alcohol, total mass fraction of the two in reaction solution is 40-60%, uses triethylamine as catalyst, is stirred at reflux
Reaction 16-24 hours removes ethyl alcohol and triethylamine, obtains polyethyleneimine functional silane coupling agent;
(2) preparation of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber
In the reactor, using ethyl alcohol as solvent, by polyethyleneimine functional silane coupling agent and ethyl orthosilicate according to matter
For amount than being uniformly mixed for 1:2-3, the mass percentage for controlling reactant is 40-60%, and basalt fibre beam is immersed in reaction
It is 1-2 with hydrochloric acid conditioning solution pH in solution, stirs 6-8 hours formation colloidal sol, adding ammonium hydroxide and adjusting pH is 9, increases temperature
To between 60-80 DEG C, 3-5 hours formation gels are stood, are freeze-dried after carrying out solvent displacement with ethyl alcohol, takes out basalt
Fibre bundle obtains polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber.
2. a kind of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction according to claim 1 is fine
The preparation method of dimension, which is characterized in that the solid-to-liquid ratio of basalt fibre beam described in step (2) and reaction solution is 1:20-30
g/mL。
3. a kind of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction according to claim 1 is fine
The preparation method of dimension, which is characterized in that concentration of hydrochloric acid described in step (2) is 1-2 mol/L.
4. a kind of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction according to claim 1 is fine
The preparation method of dimension, which is characterized in that the concentration of ammonium hydroxide described in step (2) is 1-2 mol/L.
5. a kind of polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction according to claim 1 is fine
Polyethyleneimine functionalized SiO 2 aeroge coating solid phase micro-extraction fiber prepared by the preparation method of dimension.
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Cited By (6)
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CN113185827A (en) * | 2021-04-21 | 2021-07-30 | 湖南省林业科学院 | Silicon-containing polyethyleneimine composite material and preparation method thereof |
CN113698151A (en) * | 2021-08-26 | 2021-11-26 | 安徽天锦云节能防水科技有限公司 | Polyphenyl particle-aerogel composite cement-based thermal insulation material |
CN113713723A (en) * | 2021-09-26 | 2021-11-30 | 浙江工业大学 | SiO (silicon dioxide)2@ PEI composite aerogel and preparation method and application thereof |
CN114195495A (en) * | 2020-10-17 | 2022-03-18 | 朱晶晶 | Silica aerogel composite thermal insulation fabric |
CN115677286A (en) * | 2022-11-03 | 2023-02-03 | 柳晶(溧阳)环保科技有限公司 | High-strength water permeable brick prepared from waste sand and preparation method thereof |
CN116139333A (en) * | 2023-02-28 | 2023-05-23 | 吉林大学 | Carbon fiber reinforced polyether-ether-ketone composite material and preparation method and application thereof |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114195495A (en) * | 2020-10-17 | 2022-03-18 | 朱晶晶 | Silica aerogel composite thermal insulation fabric |
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CN115677286A (en) * | 2022-11-03 | 2023-02-03 | 柳晶(溧阳)环保科技有限公司 | High-strength water permeable brick prepared from waste sand and preparation method thereof |
CN116139333A (en) * | 2023-02-28 | 2023-05-23 | 吉林大学 | Carbon fiber reinforced polyether-ether-ketone composite material and preparation method and application thereof |
CN116139333B (en) * | 2023-02-28 | 2024-04-12 | 吉林大学 | Carbon fiber reinforced polyether-ether-ketone composite material and preparation method and application thereof |
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