CN106268686A - A kind of emulsion template method prepares the method for hydrophilic macropore urea aldehyde adsorbent - Google Patents
A kind of emulsion template method prepares the method for hydrophilic macropore urea aldehyde adsorbent Download PDFInfo
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- CN106268686A CN106268686A CN201610659545.2A CN201610659545A CN106268686A CN 106268686 A CN106268686 A CN 106268686A CN 201610659545 A CN201610659545 A CN 201610659545A CN 106268686 A CN106268686 A CN 106268686A
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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
- B01J20/22—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
- B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/10—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with acyclic compounds having the moiety X=C(—N<)2 in which X is O, S or —N
- C08G12/12—Ureas; Thioureas
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
Abstract
The present invention relates to a kind of method that emulsion template method prepares macropore urea aldehyde adsorbent, belong to technical field of environment function material preparation；The present invention utilizes with carbamide and formaldehyde reaction, controls reactant pH value by triethanolamine, is prepared for urea aldehyde monomer；Secondly, with lignin as stable particle, urea aldehyde (UF) is that function monomer forms aqueous phase, with toluene as organic facies, forms pik woods High Internal Phase Emulsion；Prepare hydrophilic urea aldehyde macrocellular foam, and be applied to the absorption of phenol in aqueous solution pollutant and separate；Macroporous absorption material prepared by the present invention contains substantial amounts of macropore and connecting hole, surface hydrophilic, good penetrability and the feature containing the conjugated group such as great amount of hydroxy group, carbonyl, has good adsorption effect to phenolic comp ' ds pollution.
Description
Technical field
The present invention relates to a kind of method that emulsion template method prepares macropore urea aldehyde adsorbent, belong to environment functional material and prepare skill
Art field.
Background technology
Phenolic compound (PCs), such as nitrophenols and chlorophenol etc. are it is considered to be modal organic pollution.Containing phenol
The contaminant water of class is difficult to be degraded by microorganisms, have huge injury to natural environment, and it is 129 that U.S. Environmental Protection Agency (EPA) (EPA) is classified as
One of pollutant kind to be controlled, are also also to be a kind of harmful substance wanting priority control in China simultaneously.Accompany in recent years
Along with in industrial expansion, the discharge capacity of the sewage containing phenols and discharge water, the content of phenol is all in increase year by year.As
Most of biologies including humans are all had bigger harm by the phenolic compound of prototype matter noxious substance.Therefore, it is necessary to
A kind of effective means are found it to be removed from water body.
In recent years, multi-pore micron material because of its high porosity, low-density, high magnetic permeability and have a large amount of avtive spot and
The advantage such as easily separated is widely studied, such as activated carbon, multi-stage porous magnesium oxide, metallo-organic framework in terms of pollutant absorption
Material and poly-(glycidyl methacrylate) porous material etc..But processability is stable, pore passage structure is controlled and behaviour
The technology making convenient material is the most immature.High Internal Phase Emulsion (HIPEs), refer to internal phase (dispersion phase) volume fraction more than 74%,
A kind of short-cut method is provided by being polymerized to prepare macropore polymeric material in its foreign minister (continuous phase) initiation.Additionally, based on height
Macropore polymeric material (PloyHIPEs) prepared by internal phase emulsions includes equally and is connected with each other between many smaller hole and macropore,
Thus the material of preparation has higher porosity and the plurality of advantages such as aperture is controlled.
Can add exhibiting high surface activating agent in the preparation process of tradition High Internal Phase Emulsion, the use of surfactant can be given certainly
So Environmental security and health bring the biggest threat.Further, by the High Internal Phase Emulsion mould material that surfactant is stable
Lack enough stabilities.Pik woods High Internal Phase Emulsion template is to produce the preferable method of porous material.Use solid
Granule replaces emulsifying agent and stablizes pik woods High Internal Phase Emulsion, decreases the consumption of emulsifying agent, has saved synthesis cost, to environment
Friendly.Common solid particle is generally inorganic or polymer beads, and it is high as pik woods that the present invention have chosen lignin particles
The stable particle of internal phase emulsions.Lignin is as second-biggest-in-the-world abundant living resources, low cost, it is most important that containing suitable
When functional group can realize revising further.
The present invention is prepared for a kind of hydrophilic by oil-in-water type pik woods High Internal Phase Emulsion template based on lignin
Property macropore urea aldehyde adsorbent (UFMF), and as adsorbent with 2,4,5-trichlorophenol, 2,4,6,-Ts (2,4,5-TCP), 2,4,6-tri-
Chlorophenol (2,4,6-TCP) and 4-nitrophenol (4-NP) are the phenolic comp ' ds pollution of representative.
Summary of the invention
It is an object of the invention to overcome the stable particle of O/W type pickering emulsion traditional in prior art often to need chemistry
Modification, to guarantee that the surface wettability of stable particle be enough to obtain the defect of stable emulsion system, utilizes carbamide and formaldehyde anti-
Should, control reactant pH value by triethanolamine, be prepared for urea aldehyde monomer；Secondly, with lignin as stable particle, urea aldehyde (UF)
Form aqueous phase for function monomer, with toluene as organic facies, form pik woods High Internal Phase Emulsion；Prepare hydrophilic urea aldehyde macropore bubble
Foam, and be applied to the absorption of phenol in aqueous solution pollutant and separate.
The technical solution used in the present invention is:
(1) preparation of lignin dispersion liquid:
Different amounts of lignin is joined in a certain amount of deionized water and prepare lignin dispersion liquid, for guaranteeing that lignin can divide
Clear complete, by the pH value of dropping strong aqua ammonia regulation mixture；Then said mixture is filtered to remove impurity；Finally, filtrate
Middle dropping salt acid for adjusting pH makes lignin dispersion stable with standby.
Wherein, the concentration of prepared lignin dispersion liquid is 3.0-7.5 wt%；
The volume content of dropping strong aqua ammonia is 25%；
The pH value of described mixture is 9-11；
The pH regulating lignin dispersion liquid after described dropping hydrochloric acid is 3-5；Wherein concentration of hydrochloric acid is 1M.
(2) preparation of urea aldehyde (UF) monomer:
First, carbamide is joined formalin and is stirred by magneton, after being subsequently added triethanolamine regulation mixture ph
Stirring reaction, reacts and mixture is cooled to after terminating room temperature and dilutes with deionized water.
Wherein, the consumption of described carbamide and formalin is 12g:24.5g；Wherein, formalin concentration is 37 wt%；
Described addition triethanolamine regulation mixture pH is 8-10；
Described stirring reaction is 70 DEG C of stirring reaction 1-1.5h.
(3) preparation of hydrophilic macropore urea aldehyde adsorbent (UFMF)
First, under mechanical stirring, in round-bottomed flask urea aldehyde monomer and lignin dispersion liquid added to；Under agitation
And in aqueous phase, it is slowly added dropwise toluene as organic facies；After toluene dropping completely, stirring after adjustment of rotational speed is formed homogeneous pik
Woods High Internal Phase Emulsion template；The emulsion of formation is transferred in centrifuge tube, after polyreaction, obtains product；Then with ethanol as rope
Product is carried out washing purification, to remove the organic solvent of unreacted monomer and residual by the eluant that family name extracts；Finally, product is made
Thing UFMF is dried.
Wherein, described urea aldehyde monomer is 1.0:0.1-1.0 with the volume ratio of lignin dispersion liquid；
Described speed of agitator is 600 rpm-900rpm；
Described urea aldehyde monomer is 1.0:3-5 with the volume ratio of toluene；
After the dropping completely of described toluene, adjustment of rotational speed is 1000rpm, stirs 1.0-1.5h；
Described polyreaction is to be polymerized 24 h at 65 DEG C-75 DEG C；
Described drying condition is to be dried 24 h at 25 DEG C-40 DEG C.
Hydrophilic macropore urea aldehyde adsorbent prepared by the present invention is shelly urea formaldehyde polymer material, and pore passage structure can pass through
Controlling emulsion profit Phase Proportion and polymerization time and change, density is little, light weight.
Beneficial effects of the present invention:
The preparation process of tradition High Internal Phase Emulsion can use exhibiting high surface activating agent thus environment and human body are worked the mischief, often
See that the stable particle of pickering emulsion often needs chemical modification, to guarantee that the surface wettability of stable particle be enough to obtain stable breast
Liquid system, the biological material lignin that the present invention uses need not surface modification and aboundresources, can obtain through a step emulsion
O/W type pickering emulsion that must be stable, method is simple, with low cost.Additionally, before the macrocellular foam type adsorbent for preparing of the present invention
Driving the monomer that body is formaldehyde and urea polycondensation, raw material is simple, with low cost, and has abundant with it for adsorbent prepared by monomer
The functional group such as amino, carbonyl, can be as being effectively combined site.
The macrocellular foam type adsorbent permeability that the present invention prepares is good, porosity is high, permeability is good, and its macroporous structure can add
Strong pollutant are diffused into adsorption site through liquid medium, improve mass-transfer efficiency；Its pore passage structure can be by controlling emulsion profit
Phase Proportion and polymerization time and change, to tackle the absorption under different condition；The macrocellular foam type adsorbent density simultaneously obtained
Little, light weight, therefore the adsorption potential of unit mass is counted far above solid adsorbent.Additionally, this adsorbent surface hydrophilic is very
Good, can ensure that the dispersion that adsorbent is stable in water solution system, this feature for absorbing phenolic etc. can in water slightly soluble, can
Molten Organic substance is favourable, is therefore well suited for the adsorbing separation of organic pollution in Environmental Water solution system.
Accompanying drawing explanation
Fig. 1 is to be in a ratio of 75% (a) in pik woods High Internal Phase Emulsion, 80 (b), optical microscope time 85% (c)
Figure；In figure, scale is 10 μm.
Fig. 2 is to prepare O/W type pik woods High Internal Phase Emulsion dropping (a) and (b) in toluene in a large amount of water in embodiment 1
Result figure.
Fig. 3 is UFMF scanning electron microscope (SEM) photograph (a) of preparation in embodiment 1 and the UFMF after adsorption-desorption circulates scans
Electronic Speculum figure (b).
Fig. 4 is lignin (a) and the infrared spectrogram of UFMF (b) of preparation in embodiment 1.
Fig. 5 is lignin (a) and the contact angle of UFMF (b) of preparation in embodiment 1.
Fig. 6 is lignin (a) and the thermogravimetric analysis figure of UFMF (b) of preparation in embodiment 1.
Detailed description of the invention
In the specific embodiment of the invention, recognition performance evaluation is carried out by the following method: utilize Staticadsorption experiment complete
Become.Certain density for 10mL 2,4,5-TCP, 2,4,6TCP and 4-NP solution are joined in centrifuge tube, adds a certain amount of parent
Aqueous urea aldehyde macroporous adsorbent UFMF, is placed in 25 DEG C of constant temperature waters and stands some hours, after absorption 2,4,5-TCP, 2,4,6-
TCP and 4-NP content ultraviolet-uisible spectrophotometer measures, and calculates adsorption capacity according to result.
Below in conjunction with being embodied as example, the present invention will be further described.
Embodiment 1:
(1) preparation of lignin dispersion liquid:
The lignin of 7.5 g is joined the lignin dispersion liquid forming mass fraction 7.5 % in 92.5 mL deionized waters, for
Guarantee that lignin can disperse completely, by the pH value of dropping strong aqua ammonia (volume content 25%) regulation mixture, until pH value is
11.Then said mixture is filtered to remove impurity.Finally, dripping hydrochloric acid (1 M) regulation pH to 3 in filtrate makes lignin disperse
Liquid is stable with standby.
(2) preparation of urea aldehyde (UF) monomer:
First, 12 g carbamide joined the 37 wt% formalins of 24.5 g and is stirred by magneton, being subsequently added three ethanol
Amine regulation mixture ph is to 8.5, and 1.0h are reacted in 70 DEG C of stirrings, reacts and mixture is cooled to after terminating room temperature and goes with 50mL
Ionized water dilutes.
(3) preparation of hydrophilic macropore urea aldehyde adsorbent (UFMF):
First, under mechanical stirring, 5.4 mL urea aldehyde monomers and 0.6 mL lignin dispersion liquid (mass fraction 7.5 %) are added
In the round-bottomed flask of 100 mL.Stir under 600 rpm rotating speeds and in aqueous phase, be slowly added dropwise 24 mL toluene as organic
Phase.After toluene dropping completely, adjustment of rotational speed to 1000 rpm is stirred 1.0 hours and form homogeneous pik woods High Internal Phase Emulsion mould
Plate.The emulsion of formation is transferred in centrifuge tube, at 70 DEG C, is polymerized 24 h obtains product.Then with ethanol as surname extraction
Eluant product is carried out wash purification, to remove the organic solvent of unreacted monomer and residual.Finally, 25 DEG C of rooms
Product UFMF is made to be dried 24 h under temperature.
Fig. 2 is to prepare O/W type pik woods High Internal Phase Emulsion dropping (a) and (b) in toluene in a large amount of water in embodiment 1
Result figure.Figure (a) can be seen that after emulsion instills in water disintegration immediately, and figure (b) emulsion droplet remains to keep steady in toluene
Fixed, show successfully to prepare stable O/W type High Internal Phase Emulsion.
Fig. 3 is that in embodiment 1, UFMF scanning electron microscope (SEM) photograph (a), UFMF shown in figure of preparation contain substantial amounts of macropore and company
Connecing hole, size distribution is narrower, relatively uniform；Figure (b) is the UFMF scanning electron microscope (SEM) photograph after adsorption-desorption circulates, material
Expect that pattern does not occurs substantially to change and show that it has preferable stability.
Fig. 4 is lignin (a) and the infrared spectrogram of UFMF (b) of preparation in embodiment 1；Show successfully to prepare shelly
Urea formaldehyde polymer material.
Fig. 5 is lignin (a) and the contact angle of UFMF (b) of preparation in embodiment 1；Can be seen that lignin itself has
Good surface wettability is with stable O/W type emulsion；The UFMF material surface of preparation shows the strongest hydrophilic.
Fig. 6 is lignin (a) and the thermogravimetric analysis figure of UFMF (b) of preparation in embodiment 1；When in start temperature ranges (<
250 DEG C), UFMF and lignin weight loss substantially 10.52% and 7.15%, the most predominantly physics water suction, show that UFMF has
There is good hydrophilic；When temperature is increased to 800 DEG C, the obvious weight loss that material occurs is UFMF thermal decomposition amount, also indicates that
Material has good heat stability.
Embodiment 2:
(1) preparation of lignin dispersion liquid:
The lignin of 3.0 g is joined the lignin dispersion liquid forming mass fraction 3.0 % in 97 mL deionized waters, for really
Protect lignin and can disperse completely, by the pH value of dropping strong aqua ammonia (volume content 25%) regulation mixture, until pH value is 9.Connect
And said mixture is filtered to remove impurity.Finally, dripping hydrochloric acid (1 M) regulation pH to 5 in filtrate makes lignin dispersion liquid steady
Fixed with standby.
(2) preparation of urea aldehyde (UF) monomer:
First, 12 g carbamide joined the 37 wt% formalins of 24.5 g and is stirred by magneton, being subsequently added three ethanol
Amine regulation mixture ph is to 10, and 1.5h are reacted in 70 DEG C of stirrings, reacts and mixture is cooled to after terminating room temperature and goes with 50mL
Ionized water dilutes.
(3) preparation of hydrophilic macropore urea aldehyde adsorbent (UFMF):
First, under mechanical stirring, 5 mL urea aldehyde monomers and 5 mL lignin dispersion liquids (mass fraction 3.0 %) are added to
In the round-bottomed flask of 100 mL.Stir under 900 rpm rotating speeds and in aqueous phase, be slowly added dropwise 20 mL toluene as organic facies.
After toluene dropping completely, adjustment of rotational speed to 1000 rpm is stirred 1.5 hours and form homogeneous pik woods High Internal Phase Emulsion template.
The emulsion of formation is transferred in centrifuge tube, at 75 DEG C, is polymerized 24 h obtains product.Then washing with ethanol as surname extraction
Product is carried out washing purification, to remove the organic solvent of unreacted monomer and residual by de-agent.Finally, at 40 DEG C, product is made
Thing UFMF is dried 24 h.
Embodiment 3:
(1) preparation of lignin dispersion liquid:
The lignin of 5.0 g is joined the lignin dispersion liquid forming mass fraction 5.0 % in 95.0 mL deionized waters, for
Guarantee that lignin can disperse completely, by the pH value of dropping strong aqua ammonia (volume content 25%) regulation mixture, until pH value is
10.Then said mixture is filtered to remove impurity.Finally, dripping hydrochloric acid (1 M) regulation pH to 4 in filtrate makes lignin disperse
Liquid is stable with standby.
(2) preparation of urea aldehyde (UF) monomer:
First, 12 g carbamide joined the 37 wt% formalins of 24.5 g and is stirred by magneton, being subsequently added three ethanol
Amine regulation mixture ph to 8,70 DEG C of stirring reaction 1 h, reaction after terminating mixture is cooled to room temperature and with 50mL go from
Sub-water dilutes.
(3) preparation of hydrophilic macropore urea aldehyde adsorbent (UFMF):
First, under mechanical stirring, 4.8 mL urea aldehyde monomers and 1.2 mL lignin dispersion liquids (mass fraction 5.0 %) are added
In the round-bottomed flask of 100 mL.Stir under 800 rpm rotating speeds and in aqueous phase, be slowly added dropwise 24 mL toluene as organic
Phase.After toluene dropping completely, adjustment of rotational speed to 1000 rpm is stirred 1.5 hours and form homogeneous pik woods High Internal Phase Emulsion mould
Plate.The emulsion of formation is transferred in centrifuge tube, at 70 DEG C, is polymerized 24 h obtains product.Then with ethanol as surname extraction
Eluant product is carried out wash purification, to remove the organic solvent of unreacted monomer and residual.Finally, at 30 DEG C
Product UFMF is made to be dried 24 h.
Fig. 1 is to be in a ratio of 75% (a) in pik woods High Internal Phase Emulsion, 80 (b), optical microscope time 85% (c)
Figure；In figure, scale is 10 μm.As it can be seen, lignin can be positioned at oil-water two-phase interfaces, the emulsion formed is served very
Good Stabilization；Along with the interior rising compared, between emulsion droplet, the most crowded and drop average diameter has reduced.
Absorption property below by material prepared by the test example proof present invention.
Test example 1: respectively take 2,4,5-TCP, 2,4,6-TCP and 10mL initial concentration that 10mL initial concentration is 100mg/L
4-NP for 50mg/L is added separately in centrifuge tube, then the hydrophilic urea aldehyde macroporous absorption being separately added in 10mg embodiment 1
Agent (UFMF), is placed on test fluid in the water bath chader of 25 DEG C, respectively 5.0,15,30,60,120,240,360,480,
Take out the when of 720 min；By centrifugal, adsorbent and solution separating are opened, re-use the micropore nitric acid that aperture is 0.45mm fine
Solution is carried out filtering by dimension element film removes the particle suspended.2,4,5-TCP, 2,4,6-TCP and 4-NP in filtrate are divided by ultraviolet
Light photometer 292nm, 288 nm, 252 nm wavelength under or Atomic Absorption calculate and measure, and calculate absorption according to result
Capacity；Result shows, at initial 25min, the adsorption capacity of 2,4,5-TCP quickly increases, and this result shows 2,4,5-TCP
It is better than 2,4,6-TCP and 4-NP in UFMF diffusion into the surface speed；Additionally, UFMF is to 2, the adsorption capacity of 4,5-TCP also ratio 2,4,
6-TCP and 4-NP wants big；After quick adsorption, the rate of adsorption drastically declines and reaches balance when 1.0 h.
Test example 2: respectively take 10mL initial concentration be respectively 20,40,60,80,100 mg/L 2,4,5-trichlorophenol, 2,4,6,-T (2,
4,5-TCP), 2,4,6-trichlorophenol, 2,4,6,-Ts (2,4,6-TCP) join in centrifuge tube, take the most respectively 10mL initial concentration be respectively
10, the 4-nitrophenol (4-NP) of 20,30,40,50 mg/L add the parent in 10mg embodiment 1 to three groups of centrifuge tubes respectively
Aqueous urea aldehyde macroporous adsorbent (UFMF), after test fluid is placed in the water-bath of 25 DEG C standing 24h, supernatant high speed centrifugation
Machine separates and collects, unadsorbed 2,4,5-TCP, 2,4,6-TCP and 4-NP by ultraviolet spectrophotometer 292nm, 288 nm,
Under the wavelength of 252 nm or Atomic Absorption calculates and measures, and calculating adsorption capacity according to result, result shows, reaches absorption flat
During weighing apparatus the maximum adsorption capacity of 2,4,5-TCP, 2,4,6-TCP and 4-NP be respectively 116.3 μm ol/g, 78.74 μm ol/g and
29.4 μm ol/g, the effect of UFMF absorption 2,4,5-TCP the most more preferably, shows the type of substituted radical and position simultaneously
Adsorption effect has an impact and shows as 2,4,5-chlorine and replaces position 2,4,6-chlorine replacement position > 4-nitro replacement position.
Claims (10)
1. a macropore urea aldehyde adsorbent, it is characterised in that described adsorbent pore passage structure can be compared by controlling emulsion profit
Example and polymerization time and change, containing substantial amounts of macropore and connecting hole.
2. the preparation method of a macropore urea aldehyde adsorbent, it is characterised in that follow the steps below:
(1) preparation of lignin dispersion liquid:
Lignin is joined in deionized water and prepare lignin dispersion liquid, the pH value of dropping strong aqua ammonia regulation mixture；Then
Mixture is filtered to remove impurity；Finally, dripping salt acid for adjusting pH in filtrate makes lignin dispersion stable with standby；
(2) preparation of urea aldehyde (UF) monomer:
Carbamide joining formalin and is stirred by magneton, after being subsequently added triethanolamine regulation mixture ph, stirring is anti-
Should, react and after terminating, mixture is cooled to room temperature and dilutes with deionized water；
(3) preparation of hydrophilic macropore urea aldehyde adsorbent (UFMF):
First, under mechanical stirring, in round-bottomed flask urea aldehyde monomer and lignin dispersion liquid added to；Under agitation
And in aqueous phase, it is slowly added dropwise toluene as organic facies；After toluene dropping completely, stirring after adjustment of rotational speed is formed homogeneous pik
Woods High Internal Phase Emulsion template；The emulsion of formation is transferred in centrifuge tube, after polyreaction, obtains product；Then with ethanol as rope
Product is carried out washing purification, to remove the organic solvent of unreacted monomer and residual by the eluant that family name extracts；Finally, product is made
Thing UFMF is dried.
The preparation method of a kind of macropore urea aldehyde adsorbent the most according to claim 2, it is characterised in that institute in step (1)
The concentration of the lignin dispersion liquid stated is 3.0-7.5 wt%；The pH value of described mixture is 9-11；
The pH regulating lignin dispersion liquid after described dropping hydrochloric acid is 3-5；Wherein concentration of hydrochloric acid is 1M.
The preparation method of a kind of macropore urea aldehyde adsorbent the most according to claim 2, it is characterised in that institute in step (2)
The consumption stating carbamide and formalin is 12g:24.5g；Wherein, formalin concentration is 37 wt%；
Described addition triethanolamine regulation mixture pH is 8-10；
Described stirring reaction is 70 DEG C of stirring reaction 1-1.5h.
The preparation method of a kind of macropore urea aldehyde adsorbent the most according to claim 2, it is characterised in that institute in step (3)
The volume ratio stating urea aldehyde monomer and lignin dispersion liquid is 1.0:0.1-1.0.
The preparation method of a kind of macropore urea aldehyde adsorbent the most according to claim 2, it is characterised in that institute in step (3)
Stating speed of agitator is 600 rpm-900rpm；Described urea aldehyde monomer is 1.0:3-5 with the volume ratio of toluene.
The preparation method of a kind of macropore urea aldehyde adsorbent the most according to claim 2, it is characterised in that institute in step (3)
Stating the rear adjustment of rotational speed of toluene dropping is 1000rpm, stirs 1.0-1.5h.
The preparation method of a kind of macropore urea aldehyde adsorbent the most according to claim 2, it is characterised in that institute in step (3)
Stating polyreaction is to be polymerized 24 h at 65 DEG C-75 DEG C；Described drying condition is to be dried 24 h at 25 DEG C-40 DEG C.
9. the macropore urea aldehyde adsorbent phenol in aqueous solution pollutant described in claim 1 or 2 absorption and the application separated.
Application the most according to claim 9, it is characterised in that described phenolic comp ' ds pollution be 2,4,5-trichlorophenol, 2,4,6,-Ts, 2,
4,6-trichlorophenol, 2,4,6,-T, 4-nitrophenol.
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| CN107142255A (en) * | 2017-05-31 | 2017-09-08 | 桂林理工大学 | A kind of method of the phase pickering emulsions as templated synthesis immobilised enzymes material using in height |
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