CN108774336A - Application of the liquid metal microballoon as pore-foaming agent in preparing solid-phase extraction column - Google Patents
Application of the liquid metal microballoon as pore-foaming agent in preparing solid-phase extraction column Download PDFInfo
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- CN108774336A CN108774336A CN201810249194.7A CN201810249194A CN108774336A CN 108774336 A CN108774336 A CN 108774336A CN 201810249194 A CN201810249194 A CN 201810249194A CN 108774336 A CN108774336 A CN 108774336A
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- liquid metal
- phase extraction
- microballoon
- application according
- pore
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- 229910001338 liquidmetal Inorganic materials 0.000 title claims abstract description 46
- 238000002414 normal-phase solid-phase extraction Methods 0.000 title claims abstract description 20
- 239000004088 foaming agent Substances 0.000 title claims abstract description 13
- 229920000642 polymer Polymers 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000011148 porous material Substances 0.000 claims abstract description 9
- 238000001179 sorption measurement Methods 0.000 claims abstract description 5
- 238000010521 absorption reaction Methods 0.000 claims abstract description 3
- 239000007788 liquid Substances 0.000 claims description 16
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- 239000003431 cross linking reagent Substances 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- -1 methyl acrylic ester Chemical class 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 6
- 229910052733 gallium Inorganic materials 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000010334 sieve classification Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000005199 ultracentrifugation Methods 0.000 claims description 5
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- 229910052738 indium Inorganic materials 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 239000012071 phase Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 239000011324 bead Substances 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 3
- 229920002521 macromolecule Polymers 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 239000002861 polymer material Substances 0.000 claims description 3
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 3
- 229920000053 polysorbate 80 Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- 230000003213 activating effect Effects 0.000 claims description 2
- 238000004220 aggregation Methods 0.000 claims description 2
- 230000002776 aggregation Effects 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 229920000058 polyacrylate Polymers 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- 238000012546 transfer Methods 0.000 claims description 2
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 claims 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000003960 organic solvent Substances 0.000 abstract description 3
- 231100000331 toxic Toxicity 0.000 abstract description 3
- 230000002588 toxic effect Effects 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 230000006872 improvement Effects 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229920001730 Moisture cure polyurethane Polymers 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000002925 chemical effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000006854 communication Effects 0.000 description 1
- 230000002508 compound effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000010829 isocratic elution Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- 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
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
-
- 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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3064—Addition of pore forming agents, e.g. pore inducing or porogenic agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/1006—Esters of polyhydric alcohols or polyhydric phenols
- C08F222/102—Esters of polyhydric alcohols or polyhydric phenols of dialcohols, e.g. ethylene glycol di(meth)acrylate or 1,4-butanediol dimethacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2335/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical, and containing at least one other carboxyl radical in the molecule, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Derivatives of such polymers
- C08J2335/02—Characterised by the use of homopolymers or copolymers of esters
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- Chemical & Material Sciences (AREA)
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- Polymers & Plastics (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
Application the invention discloses liquid metal microballoon as pore-foaming agent in preparing solid-phase extraction column.The Solid Phase Extraction adsorbing separation high molecular material for the controllable bore diameter and porosity that this method is prepared has the following advantages：1. the adsorbing separation high molecular material being prepared can be according to the characteristic of target compound, the pore size and porosity of arbitrary regulation and control polymer make it possess the absorption hole to match with adsorbing separation subject molecule size and diffusion admittance.2. polymeric inner opening structure is uniform, favorable reproducibility.With the characteristic for higher column effect and quick adsorption can be carried out detaching.3. having reached green recycling instead of the organic solvent pore-foaming agent of conventional toxic high pollution with the liquid metal droplet of nanometer and micron diameter.
Description
Technical field
The present invention relates to the preparation of polymeric solid phase extraction column and applications, and in particular to liquid metal microballoon is as pore-foaming agent
Application in preparing solid-phase extraction column.
Background technology
In recent years, liquid metal oneself become modern material processing research hotspot, be used as sensing material, plastics and urge
Agent etc..Especially gallium and gallium-indium liquid alloy, their fusing point are 29.8 DEG C, are deformable, shaping, can note
The metal penetrated.There is strong correlation between the performance of liquid metal and structure feature, therefore, controls its granular size, shape
It is just very necessary with structure.
By modes such as heat treatment, electron beam irradiation or pressurizations, preforming liquid metal nano particle fusion can induce
The shape different with being converted to, such as linear, triangle or spongy.Ultrasonic wave is a kind of mechanical wave in elastic fluid.Power
Ultrasound is used as a kind of form of energy, can influence or change the property of medium.In its communication process, mainly have to the effect of medium
Three aspect of temperature action, mechanical agitation and cavitation.Physical effect that ultrasonic cavitation is caused, mechanical effect, thermal effect
It answers, biological effect, chemical effect etc. industrially have wide application potential.Using ultrasonic wave in refinement and hookization group
Knit, eliminate the remarkable effect of wetability etc. between gravity segregation and improvement molten metal ceramics.
It prepares in the prior art in the high-molecular porous materials process of adsorbing separation analysis and mostly uses having for toxic high pollution
Solvent is influenced and restriction in the course of the polymerization process by polymerizing condition, organic solvent pore-foaming agent and function monomer and crosslinking agent
The polymer of formation is separated, and the uncontrollable significant difference hole of diversity is presented in the high molecular material aperture obtained from
The present situation of road distribution.
Invention content
In order to solve the deficiencies in the prior art, the present invention provides liquid metal microballoon as pore-foaming agent in preparation solid phase extraction
Take the application in column.
The technical scheme is that：Application of the liquid metal microballoon as pore-foaming agent in preparing solid-phase extraction column.
Further improvement of the present invention includes：
The liquid metal is gallium or gallium-indium liquid alloy.
The preparation method of the solid-phase extraction column is as follows：Liquid metallic microspheres are prepared, using methyl acrylic ester as work(
Energy monomer, ethylene glycol dimethacrylate is crosslinking agent, molar ratio 1:4~1:6；Addition accounts for function monomer and crosslinking agent
The liquid metal microballoon of total volume 30%~60%, and the preparation of photoinitiator 1800 for accounting for function monomer quality 1%~3% is added
Polyacrylate Solid Phase Extraction adsorption stuffing；Obtained macromolecule polymer material is taken out, is ground in the agate mortar
It is broken；Taylor's sieve classification is crossed, takes grain size spare in 30 μm~70 μm of particulate polymers；By the particulate polymers after sieve classification
Removal liquid metal droplet obtains the high-molecular porous material of adsorbing separation of controllable bore diameter and porosity；It can by what is be prepared
The high-molecular porous mixture of adsorbing separation of aperture and porosity is controlled in solid up to esters of acrylic acid in blank pipe solid phase extraction tube
Phase extraction column.Nitrogen is first passed through before polymerisation into mixed solution 15 minutes, to remove the dissolved oxygen in pre-polymer solution；Again
Mixed solution is injected after capillary and places 12h in 60 DEG C of hot bath, free radical in situ polymerization reaction occurs.
The methyl acrylic ester is that function monomer is 2- methacrylic acids, butyl methacrylate, metering system
Sour isobutyl ester and/or hydroxyethyl methacrylate.
The preparation method of the liquid metal microballoon is as follows：By liquid metal and surfactant in dispersed phase isopropanol
According to mass ratio 1:0.2：1 amount mixing, is ultrasonically treated, obtains dispersed liquid state molten drop later, will prepare the dispersion of gained
Liquid metal droplet carries out ultracentrifugation (25000rpm), after centrifuging 15 minutes, extracts removal supernatant, retains bottom deposit
Object adds isopropanol, centrifuges under these conditions, removes supernatant, which is repeated 3 times, to remove extra table
Face activating agent, then (- 40 DEG C) freeze-dryings of low temperature obtain liquid metal microsphere powder, are placed on spare in low temperature refrigerator；Institute
It states surfactant and is wrapped in liquid metal droplets surface, liquid metal surface tension can be made to be remarkably decreased, and the gold to be formed can be made
Belong to drop solution surface orientation aligned transfer, in 20 DEG C of ultrasonic procedures, gallium (29.8 DEG C of fusing point) and gallium-indium mixes liquid
Metal (29.8 DEG C of fusing point) remains to keep liquid, while the viscosity of temperature influence isopropanol, excessively high temperature can make isopropanol
Viscosity reduces.By four amount of surfactant, temperature, ultrasonic power and time factor co- controlling liquid metal droplet diameters
Size.
The surfactant is Tween 80, Span 80, that bent logical 100, cetyl trimethylammonium bromide and/or 12
Sodium alkyl sulfate.
Temperature is 15~50 DEG C when the supersound process；The ultrasonic power is 50~200W.
A diameter of 250nm~1200nm of the liquid metal microballoon.
The preparation method of the integral post further includes removal liquid metal microballoon as follows, specifically includes particulate polymers dispersion
Into the aqueous solution of saline media, then positive and negative platinum electrode is inserted into solution, connection DC power supply, control voltage 30V~
120V, electric current 0.01mA~0.5mA；It is aided with 40 DEG C of water bath ultrasonic wave to the aqueous solution for being dispersed with particulate polymers simultaneously, carries
It removes except the liquid metal droplet in polymer beads；Extraction 20 minutes every time, repeat above procedure 3~6 times, reach and go completely
Except liquid metal droplet；Aqueous solution after the extraction recovering liquid molten drop after ultracentrifugation filters.
The Solid Phase Extraction adsorbing separation high molecular material for the controllable bore diameter and porosity that this method is prepared has following
Advantage：1. the adsorbing separation high molecular material being prepared can be according to the characteristic of target compound, the hole of arbitrary regulation and control polymer
Diameter size and porosity make it possess the absorption hole to match with adsorbing separation subject molecule size and diffusion admittance.2. poly-
It is uniform to close object internal cavity structure, favorable reproducibility.With the characteristic for higher column effect and quick adsorption can be carried out detaching.3. to receive
The liquid metal droplet of rice and micron diameter has reached green repetition instead of the organic solvent pore-foaming agent of conventional toxic high pollution
It utilizes.
The present invention is proposed can to prepare as green pore-foaming agent using controllable nanometer and micron low temperature liquid molten drop
The adsorbing separation of control aperture and specific surface area analyzes high-molecular porous material preparation method and applies it to actual complex sample
In pretreatment process.
Description of the drawings
For Fig. 1 to be of the invention with liquid metal microballoon transmission scanning electron microscope figure made from embodiment 1, scale is 200 nanometers.
Fig. 2 is that the present invention elutes liquid metallic microspheres post-consumer polymer scanning electron microscope (SEM) photograph so that embodiment 1 is obtained, and scale is
5 microns.
Specific implementation mode
It elaborates to the present invention with reference to embodiment.
Embodiment 1
Using liquid metal microballoon gallium as pore-foaming agent, the Tween 80 of the gallium of 0.5g and 0.1g is added in the isopropanol of 5mL,
Controlled at 20 DEG C, ultrasonic power 150W, point that particle size range is 250nm~1200nm is prepared in ultrasound 30 minutes
Dissipate liquid metal droplet.
The dispersed liquid state molten drop for preparing gained is subjected to ultracentrifugation (25000rpm), after centrifuging 15 minutes, is taken out
It removes and removes supernatant, retain basic sediment.The operation is repeated 3 times, to remove extra surfactant.Low temperature cold again
Dry (- 40 DEG C) are lyophilized and obtain liquid metal microsphere powder.It places it in low temperature refrigerator (- 10 DEG C) and saves backup.
Using methacrylic acid as function monomer, ethylene glycol dimethacrylate is crosslinking agent, and its ratio be 1:4.It is added
The liquid metal microballoon of function monomer and crosslinking agent total volume 50% is accounted for, and is added and accounts for function monomer and crosslinking agent gross mass 2%
Photoinitiator 1800 prepare Solid Phase Extraction adsorption stuffing.Nitrogen is first passed through before polymerisation into mixed solution 15 minutes, with
Remove the dissolved oxygen in pre-polymer solution；It polymerize 20min under ultraviolet lighting after mixed solution is sealed in ampere bottle again to obtain
To blocky high molecular polymer.
Obtained macromolecule polymer material is taken out, Taylor's sieve classification is crossed after grinding is broken, take grain size 30 μm~
70 μm of particulate polymers are spare.Particulate polymers after sieve classification are distributed in the aqueous solution of saline media, then to molten
It is inserted into positive and negative platinum electrode in liquid, connects DC power supply, controls voltage 60V, electric current 0.03mA.Simultaneously to being dispersed with aggregation of particles
The aqueous solution of object is aided with 40 DEG C of water bath ultrasonic wave, the liquid metal droplet in extraction removal polymer beads.Extraction 20 every time
Minute, it repeats above procedure 6 times, reaches and completely remove liquid metal droplet.Aqueous solution after extraction passes through ultracentrifugation mistake
Recovering liquid molten drop after filter.Obtain the high-molecular porous material of adsorbing separation of controllable bore diameter and porosity.
By the high-molecular porous material of the adsorbing separation of the controllable bore diameter being prepared and porosity, removed with soxhlet extraction methods
Unreacted pore-foaming agent etc., extraction solvent are methanol, and the time is for 24 hours that filler is dried in vacuo 6h at 60 DEG C after extracting.
The high-molecular porous material for preparing gained is applied to the sample (water) of actual sample concentration and separation target compound
Pre-treatment.It takes 100mg above-mentioned and is loaded in the blank pipe solid phase extraction tube of 3mL with the porous material that methanol cleaned, SPE pillars
Top and bottom are respectively put into polypropylene sieve plate.Before loading, SPE pillars use the deionized water balance of 10mL methanol and 5mL respectively；
With the pH to 6.0 of 0.1mol/LHCl or 0.1mol/L NaOH tune samples to be tested, with the flow velocity loading of 1mL/min；After loading, first
SPE pillars are eluted with the deionized water of 2mL, then vacuum pump is drained, and finally 5mL acetonitriles is used to elute.Eluent is blown through nitrogen
After solvent is removed in cleaning, 1mL is settled to using acetonitrile-water (6: 4, v/v) mixed liquor, is carried out after 0.45 μm of organic membrane filtration high
Effect liquid phase chromatogram (HPLC) is analyzed.
Liquid phase chromatogram condition
1260 LC chromatographic systems of Agilent.C18 columns (5 μm, 250mm × 4.6mm i.d.).Mobile phase：For acetonitrile (A)
With water (B), isocratic elution (A:B=35:65).Flow is 1.0mL min-1, 10 μ L, UV wavelength 323nm of sample size.
1 extraction column enriched compound effect of table
Those skilled in the art can be accurate according to other technological parameters described in explanation under the guidance of the present embodiment
Therefore in order to save examination resource, other embodiment is not listed in errorless reproduction the technical program.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (9)
1. application of the liquid metal microballoon as pore-foaming agent in preparing solid-phase extraction column.
2. application according to claim 1, which is characterized in that the liquid metal is gallium or gallium-indium liquid alloy.
3. application according to claim 1 or 2, which is characterized in that the preparation method of the solid-phase extraction column is as follows：System
Standby liquid metal microballoon；Using methyl acrylic ester as function monomer, ethylene glycol dimethacrylate is crosslinking agent, mole
Than being 1:4~1:6；The liquid metal microballoon for accounting for function monomer and crosslinking agent total volume 30%~60% is added, and is added and accounts for work(
The photoinitiator of energy monomer mass 1%~3% prepares polyacrylate Solid Phase Extraction adsorption stuffing；By obtained macromolecule
Polymer material takes out, and grinding is broken in the agate mortar；Taylor's sieve classification is crossed, aggregation of particles of the grain size at 30 μm~70 μm is taken
Object is spare；It is to obtain the absorption point of controllable bore diameter and porosity by the particulate polymers removal liquid metal droplet after sieve classification
From high-molecular porous material；By the high-molecular porous mixture of the adsorbing separation of the controllable bore diameter being prepared and porosity in sky
Up to esters of acrylic acid solid-phase extraction column in solid phase extraction tube.
4. application according to claim 3, which is characterized in that the methyl acrylic ester is that function monomer is 2- first
Base acrylic acid, butyl methacrylate, Isobutyl methacrylate and/or hydroxyethyl methacrylate.
5. application according to claim 3, which is characterized in that the preparation method of the liquid metal microballoon is as follows：By liquid
State metal is with surfactant according to mass ratio 1 in dispersed phase isopropanol:0.2：1 amount mixing, is ultrasonically treated, obtains later
The dispersed liquid state molten drop for preparing gained is carried out ultracentrifugation, after centrifuging 15 minutes, extracted by dispersed liquid state molten drop
Supernatant is removed, retains basic sediment, adds isopropanol, centrifuges under these conditions, remove supernatant, the operation is repeatedly
It carries out 3 times, to remove extra surfactant, then frozen drying obtains liquid metal microsphere powder；The surface
Activating agent is wrapped in liquid metal droplets surface, liquid metal surface tension can be made to be remarkably decreased, and can make the molten drop to be formed
In the surface orientation aligned transfer of solution.
6. application according to claim 5, which is characterized in that the surfactant is Tween 80, Span 80, Qu Natong
100, cetyl trimethylammonium bromide and/or lauryl sodium sulfate.
7. application according to claim 5, which is characterized in that temperature is 15~50 DEG C when the supersound process；It is described super
Acoustical power is 50~200W.
8. application according to claim 3, which is characterized in that a diameter of 250nm of the liquid metal microballoon~
1200nm。
9. application according to claim 3, which is characterized in that the preparation method of the solid-phase extraction column further includes as follows
It except liquid metal microballoon, specifically includes particulate polymers and is distributed in the aqueous solution of saline media, then be inserted into solution positive and negative
Platinum electrode connects DC power supply, controls voltage 30V~120V, electric current 0.01mA~0.5mA；It is poly- to being dispersed with particle simultaneously
The aqueous solution for closing object is aided with 40 DEG C of water bath ultrasonic wave, the liquid metal droplet in extraction removal polymer beads；Extraction every time
It 20 minutes, repeats above procedure 3~6 times, reaches and completely remove liquid metal droplet；Aqueous solution after extraction by ultrahigh speed from
Recovering liquid molten drop after heart filtering.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090105451A1 (en) * | 2007-10-22 | 2009-04-23 | Shukla Ashok K | Use of aqueous wettable hydrophobic chromatographic media for the purification of peptides, and other biomolecules |
| CN103721707A (en) * | 2012-10-15 | 2014-04-16 | 通用汽车环球科技运作有限责任公司 | Preparation of hollow pt and pt-alloy catalysts |
| CN103869013A (en) * | 2014-03-18 | 2014-06-18 | 河北出入境检验检疫局检验检疫技术中心 | Online purification solid-phase extraction monolithic column and preparation method and purposes of monolithic column |
| CN104001347B (en) * | 2014-05-13 | 2015-09-30 | 齐鲁工业大学 | A kind of preparation method of hydrophily wide spectrum solid-phase extraction column |
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2018
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090105451A1 (en) * | 2007-10-22 | 2009-04-23 | Shukla Ashok K | Use of aqueous wettable hydrophobic chromatographic media for the purification of peptides, and other biomolecules |
| CN103721707A (en) * | 2012-10-15 | 2014-04-16 | 通用汽车环球科技运作有限责任公司 | Preparation of hollow pt and pt-alloy catalysts |
| CN103869013A (en) * | 2014-03-18 | 2014-06-18 | 河北出入境检验检疫局检验检疫技术中心 | Online purification solid-phase extraction monolithic column and preparation method and purposes of monolithic column |
| CN104001347B (en) * | 2014-05-13 | 2015-09-30 | 齐鲁工业大学 | A kind of preparation method of hydrophily wide spectrum solid-phase extraction column |
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