CN109173983A - A method of hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber is prepared in situ - Google Patents
A method of hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber is prepared in situ Download PDFInfo
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- CN109173983A CN109173983A CN201810888753.9A CN201810888753A CN109173983A CN 109173983 A CN109173983 A CN 109173983A CN 201810888753 A CN201810888753 A CN 201810888753A CN 109173983 A CN109173983 A CN 109173983A
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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
- B01J20/28047—Gels
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Abstract
The invention discloses a kind of methods that hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber is prepared in situ, in particular to the chemical reaction that hybridization of ionic liquid aerosil is prepared in situ is participated in using the hydroxyl of titanium dioxide nano-rod.This new method is characterized in that first being provided for hydroxy functional group in titanium silk table wheat flour for titanium dioxide nano-rod；The ionic liquid of preparation contains methoxy silane end moieties, is chemically bonded while hydrolysis with ethyl orthosilicate hydridization with titanium hydroxyl, hybridization of ionic liquid aerosil coating has been prepared in situ in titanium silk table face.Hybridization of ionic liquid aerosil coated titanium silk solid-phase micro-extraction fibre prepared by the present invention has many advantages, such as that high mechanical strength, coating stability are good, loading capacity is high, extraction selectivity is good, food analysis, environmental analysis, in terms of have good application potential.
Description
Technical field
The present invention relates to a kind of hybridization of ionic liquid aerosil coating solid phase micro-extraction fibers of being prepared in situ
Technology.
Background technique
Solid phase micro-extraction technique is a kind of novel sample pre-treatments and beneficiation technologies risen the 1990s, is belonged to non-
Solvent type selective extraction method, be it is a kind of grow up in solid phase extraction techniques collect sampling, extraction, concentration and sample introduction in one
The micro-extraction new technology of body, and have many advantages, such as easy to operate, easy to carry, low-cost.Currently, in every field such as ring
Border, biology, industry, food, clinical medicine etc., solid phase microextraction have been developed as most commonly used Sample Pretreatment Technique side
One of method.The core component of solid phase microextraction is extracting fiber, and commercialization solid-phase micro-extraction fibre is primarily present coating extraction effect
The disadvantages of rate is low, stability is poor and bad mechanical strength, it is difficult to meet practical application request, develop the fibre of high-performance extraction coating
Dimension is still the important development direction in solid phase microextraction field.
Aeroge be it is a kind of be cross-linked with each other by colloidal particle or polymer molecule constitute have three-dimensional space network structure
Nano-meter porous amorphous lightweight solid material, it is internal containing a large amount of micron order and nanoscale cavity, significantly increase
Specific surface area.The excellent absorption property that aeroge is shown exactly shows that its huge research in solid phase microextraction field is latent
Power.But inorganic aerogels bad mechanical strength, organic aerogel heat resistance is poor, seriously restricts the extensive use of aeroge.
The fuse salt that ionic liquid is made of the biggish organic cation of volume and inorganic or inorganic anion has only
Special physicochemical properties, such as fusing point is low, thermal stability is good, extraction ability is excellent, can provide include hydrophobic, hydrogen bond, π-π,
Multi-solvents interaction type including n- π, dipole, ion/charge etc. is the research of environment in recent years analysis field and application
One of most new material.It is modified with hybridization of ionic liquid aerosil, what ionic liquid contained has
Machine functional group can not only improve the shortcomings that aeroge bad mechanical strength, can also improve its extraction ability.
Summary of the invention
The purpose of the present invention is to provide one kind, that hybridization of ionic liquid aerosil coating solid phase is prepared in situ is micro-
The technology of extracting fiber.The present invention is based on the hydroxyl participations of titanium dioxide nano-rod to prepare hybridization of ionic liquid silica airsetting
Ion liquid modified aerosil coating has been prepared in situ in titanium silk table face in the chemical reaction of glue, it is characterised in that should
Method has following processing step:
In mass ratio be 1:(8-10 by bipyridinium ion liquid, ethyl orthosilicate, ethyl alcohol and water): (10-12): (3-5) into
Row mixing, obtains mixed solution after mixing evenly, and it is 2-3 that hydrochloric acid control mixed solution pH, which is added, and titanium dioxide nano-rod is repaired
The titanium silk of decorations is immersed in reaction solution, is reacted 4-8 hours between 80-100 DEG C, and addition ammonium hydroxide tune pH is 7-8, stands 12-
The taking-up of titanium silk is freeze-dried after 18 hours, it is fine to obtain hybridization of ionic liquid aerosil coating solid phase micro-extraction
Dimension.
The present invention was prepared in situ in the step of hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber
The bipyridinium ion liquid be reacted as 4,4- bipyridyl with bromopropyl trimethoxy silane made from.
The present invention was prepared in situ in the step of hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber
The titanium silk of titanium dioxide nano-rod modification be as butyl titanate made from the calcining of titanium silk table face.
The solid-phase micro-extraction fibre of hybridization of ionic liquid aerosil coating of the present invention has following
Advantage:
(1) titanium dioxide nano-rod fabricated in situ not only provided bond groups but also had been that aeroge plays the role of bracket；
(2) hydridization of ionic liquid makes aerosil improve extraction efficiency while improving mechanical strength.
Detailed description of the invention
Fig. 1 is the preparation reaction schematic diagram of ionic liquid.
Fig. 2 is that hybridization of ionic liquid aerosil prepares schematic diagram.
Specific embodiment
For a better understanding of the present invention, it is illustrated by example:
Embodiment 1:
In mass ratio it is that 1:8:10:3 is mixed by bipyridinium ion liquid, ethyl orthosilicate, ethyl alcohol and water, stirs evenly
After obtain mixed solution, it is 2-3 that hydrochloric acid control mixed solution pH, which is added, and the titanium silk that titanium dioxide nano-rod is modified is immersed in instead
It answers in solution, is stirred to react at 80 DEG C 6 hours, addition ammonium hydroxide tune pH is 7-8, freezes the taking-up of titanium silk after standing 12 hours
It is dry, obtain hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber.
Embodiment 2:
In mass ratio it is that 1:9:10:4 is mixed by bipyridinium ion liquid, ethyl orthosilicate, ethyl alcohol and water, stirs evenly
After obtain mixed solution, it is 2-3 that hydrochloric acid control mixed solution pH, which is added, and the titanium silk that titanium dioxide nano-rod is modified is immersed in instead
It answers in solution, is reacted 5 hours between 90 DEG C, addition ammonium hydroxide tune pH is 7-8, freezes the taking-up of titanium silk after standing 14 hours
It is dry, obtain hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber.
Embodiment 3:
It is in mass ratio that 1:10:12:5 is mixed by bipyridinium ion liquid, ethyl orthosilicate, ethyl alcohol and water, stirring is equal
Mixed solution is obtained after even, it is 2-3 that hydrochloric acid control mixed solution pH, which is added, and the titanium silk that titanium dioxide nano-rod is modified is immersed in
It in reaction solution, is reacted 4 hours between 100 DEG C, addition ammonium hydroxide tune pH is 7-8, takes out titanium silk after standing 16 hours and carries out
Freeze-drying, obtains hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber.
Embodiment 4:
It is in mass ratio that 1:10:10:5 is mixed by bipyridinium ion liquid, ethyl orthosilicate, ethyl alcohol and water, stirring is equal
Mixed solution is obtained after even, it is 2-3 that hydrochloric acid control mixed solution pH, which is added, and the titanium silk that titanium dioxide nano-rod is modified is immersed in
It in reaction solution, is reacted 3 hours between 100 DEG C, addition ammonium hydroxide tune pH is 7-8, takes out titanium silk after standing 18 hours and carries out
Freeze-drying, obtains hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber.
Claims (4)
1. a kind of method that hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber is prepared in situ, feature exist
In being in mass ratio 1:(8-10 by bipyridinium ion liquid, ethyl orthosilicate, ethyl alcohol and water): (10-12): (3-5) is carried out
Mixing obtains mixed solution after mixing evenly, and it is 2-3 that hydrochloric acid control mixed solution pH, which is added, and titanium dioxide nano-rod is modified
Titanium silk be immersed in reaction solution, be stirred to react between 80-100 DEG C 3-6 hours, addition ammonium hydroxide tune pH be 7-8, stand
The taking-up of titanium silk is freeze-dried after 12-18 hours, obtains the micro- extraction of hybridization of ionic liquid aerosil coating solid phase
Take fiber.
2. hybridization of ionic liquid aerosil coating solid phase micro-extraction is prepared in situ in one kind according to claim 1
The method of fiber, which is characterized in that bipyridinium ion liquid is by 4,4- bipyridyl and the bromopropyl trimethoxy silane system of reacting
?.
3. hybridization of ionic liquid aerosil coating solid phase micro-extraction is prepared in situ in one kind according to claim 1
The method of fiber, which is characterized in that the titanium silk of titanium dioxide nano-rod modification is to be calcined to make in titanium silk table face by butyl titanate
?.
4. hybridization of ionic liquid aerosil coating solid phase micro-extraction is prepared in situ in one kind according to claim 1
Hybridization of ionic liquid aerosil coating solid phase micro-extraction fiber prepared by the method for fiber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810888753.9A CN109173983B (en) | 2018-08-07 | 2018-08-07 | Method for in-situ preparation of ionic liquid hybrid silica aerogel coating solid-phase micro-extraction fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810888753.9A CN109173983B (en) | 2018-08-07 | 2018-08-07 | Method for in-situ preparation of ionic liquid hybrid silica aerogel coating solid-phase micro-extraction fiber |
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| Publication Number | Publication Date |
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| CN109173983A true CN109173983A (en) | 2019-01-11 |
| CN109173983B CN109173983B (en) | 2021-07-27 |
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| CN201810888753.9A Active CN109173983B (en) | 2018-08-07 | 2018-08-07 | Method for in-situ preparation of ionic liquid hybrid silica aerogel coating solid-phase micro-extraction fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112808227A (en) * | 2020-12-28 | 2021-05-18 | 苏州启创新材料科技有限公司 | Hybrid aerogel adsorbent, preparation method thereof and application of hybrid aerogel adsorbent in wastewater treatment |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468306A (en) * | 2007-12-29 | 2009-07-01 | 中国科学院生态环境研究中心 | Titanium-containing solid phase micro-extraction head and preparation method thereof |
| CN102600816A (en) * | 2012-03-23 | 2012-07-25 | 济南大学 | Preparation method of solid-phase microextraction fibers by bonding metal wire with polyion liquid |
| CN106475075A (en) * | 2015-08-31 | 2017-03-08 | 中国石油化工股份有限公司 | A kind of preparation method of Nano tube array of titanium dioxide base solid-phase micro-extraction fibre |
-
2018
- 2018-08-07 CN CN201810888753.9A patent/CN109173983B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468306A (en) * | 2007-12-29 | 2009-07-01 | 中国科学院生态环境研究中心 | Titanium-containing solid phase micro-extraction head and preparation method thereof |
| CN102600816A (en) * | 2012-03-23 | 2012-07-25 | 济南大学 | Preparation method of solid-phase microextraction fibers by bonding metal wire with polyion liquid |
| CN106475075A (en) * | 2015-08-31 | 2017-03-08 | 中国石油化工股份有限公司 | A kind of preparation method of Nano tube array of titanium dioxide base solid-phase micro-extraction fibre |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112808227A (en) * | 2020-12-28 | 2021-05-18 | 苏州启创新材料科技有限公司 | Hybrid aerogel adsorbent, preparation method thereof and application of hybrid aerogel adsorbent in wastewater treatment |
| CN112808227B (en) * | 2020-12-28 | 2023-09-19 | 苏州城市学院 | Hybrid aerogel adsorbent, preparation method thereof and application thereof in wastewater treatment |
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| CN109173983B (en) | 2021-07-27 |
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Inventor after: Sun Min Inventor after: Feng Juanjuan Inventor after: Tian Yu Inventor after: Wang Xiuqin Inventor before: Tian Yu Inventor before: Sun Min Inventor before: Feng Juanjuan Inventor before: Wang Xiuqin |
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