CN106268686B - A kind of method of emulsion template method preparation hydrophily macropore ureaformaldehyde adsorbent - Google Patents

A kind of method of emulsion template method preparation hydrophily macropore ureaformaldehyde adsorbent Download PDF

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CN106268686B
CN106268686B CN201610659545.2A CN201610659545A CN106268686B CN 106268686 B CN106268686 B CN 106268686B CN 201610659545 A CN201610659545 A CN 201610659545A CN 106268686 B CN106268686 B CN 106268686B
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ureaformaldehyde
macropore
adsorbent
lignin
monomer
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CN106268686A (en
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刘金鑫
潘建明
顾润兴
白雪
张文莉
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Jiangsu University
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Jiangsu University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/268Polymers created by use of a template, e.g. molecularly imprinted polymers
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G12/00Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
    • C08G12/02Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
    • C08G12/04Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
    • C08G12/10Condensation 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
    • C08G12/12Ureas; Thioureas
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • C02F2101/345Phenols

Abstract

The present invention relates to a kind of methods that emulsion template method prepares macropore ureaformaldehyde adsorbent, belong to technical field of environment function material preparation;The present invention is utilized to be reacted with urea and formaldehyde, is controlled reactant pH value by triethanolamine, is prepared for ureaformaldehyde monomer;Secondly, ureaformaldehyde (UF) is that function monomer forms water phase using lignin as stable particle, using toluene as organic phase, pik woods High Internal Phase Emulsion is formed;Prepare hydrophily ureaformaldehyde macrocellular foam, and be applied to the absorption of phenol in aqueous solution pollutant with separate;Macroporous absorption material prepared by the present invention contains a large amount of macropore and connecting hole, surface hydrophilic, good penetrability and the characteristics of containing conjugated groups such as great amount of hydroxy group, carbonyls, has good adsorption effect to phenolic comp ' ds pollution.

Description

A kind of method of emulsion template method preparation hydrophily macropore ureaformaldehyde adsorbent
Technical field
The present invention relates to a kind of methods that emulsion template method prepares macropore ureaformaldehyde adsorbent, belong to environment functional material and prepare skill Art field.
Background technique
Phenolic compound (PCs), such as nitrophenols and chlorophenol etc., it is considered to be the most common organic pollutant.Contain phenol The contaminant water of class is difficult to be degraded by microorganisms, has huge injury to natural environment, it is 129 that Environmental Protection Agency (EPA) is classified as Kind one of the pollutant preferentially to be controlled, while and being also a kind of harmful substance for wanting priority control in China.Companion in recent years With the development of industry, the content of phenol is all in increase year by year in the discharge amount of the sewage containing phenols and discharge water.As The phenolic compound of prototype matter noxious material all has biggish harm to most of biologies including humans.Therefore, it is necessary to A kind of effective means are found to remove it from water body.
In recent years, multi-pore micron material because its high porosity, low-density, high magnetic permeability and have a large amount of active sites and The advantages that easily separated, is widely studied in terms of pollutant absorption, such as active carbon, multi-stage porous magnesia, metallo-organic framework Material and poly- (glycidyl methacrylate) porous material etc..However processability is stable, cellular structure is controllable and grasps The technology for making convenient material is still immature.High Internal Phase Emulsion (HIPEs), refer to interior phase (dispersed phase) volume fraction 74% or more, A kind of short-cut method is provided by causing to be polymerized to prepare macropore polymeric material in its foreign minister's (continuous phase).In addition, based on height The macropore polymeric material (PloyHIPEs) of internal phase emulsions preparation is equally connected with each other between smaller hole and macropore comprising there are many, Many advantages, such as material porosity with higher thus prepared and controllable aperture.
Exhibiting high surface activating agent can be added in the preparation process of traditional High Internal Phase Emulsion, the use of surfactant can be to certainly Right Environmental security and human health bring very big threat.Also, 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 ideal method of porous material.Use solid Particle replaces emulsifier to stablize pik woods High Internal Phase Emulsion, reduces the dosage of emulsifier, has saved synthesis cost, to environment It is friendly.Common solid particle is generally inorganic or polymer beads, and it is high as pik woods that the present invention has chosen lignin particles The stable particle of internal phase emulsions.Lignin is as second-biggest-in-the-world living resources abundant, low cost, it is most important that containing suitable When functional group can realize further modification.
It is prepared in the present invention by the oil-in-water type pik woods High Internal Phase Emulsion template based on lignin a kind of hydrophilic Property macropore ureaformaldehyde adsorbent (UFMF), and adsorb 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 the prior art often to need chemistry It is modified, it is anti-using urea and formaldehyde to ensure that the surface wettability of stable particle is enough to obtain the defect of stable emulsion system It answers, reactant pH value is controlled by triethanolamine, is prepared for ureaformaldehyde monomer;Secondly, using lignin as stable particle, ureaformaldehyde (UF) Water phase is formed for function monomer, using toluene as organic phase, forms pik woods High Internal Phase Emulsion;Prepare hydrophily ureaformaldehyde macropore bubble Foam, and be applied to the absorption of phenol in aqueous solution pollutant with separate.
The technical solution adopted by the present invention is that:
(1) preparation of lignin dispersion liquid:
Different amounts of lignin is added in a certain amount of deionized water and prepares lignin dispersion liquid, to ensure lignin It can disperse completely, to pass through and the pH value that concentrated ammonia liquor adjusts mixture is added dropwise;Then said mixture is filtered to remove impurity;Finally, Salt acid for adjusting pH is added dropwise in filtrate makes lignin dispersion stable with spare.
Wherein, the concentration of prepared lignin dispersion liquid is 3.0-7.5 wt%;
The volume content that concentrated ammonia liquor is added dropwise is 25%;
The pH value of the mixture is 9-11;
The pH that lignin dispersion liquid is adjusted after the dropwise addition hydrochloric acid is 3-5;Wherein concentration of hydrochloric acid is 1M.
(2) preparation of ureaformaldehyde (UF) monomer:
Firstly, urea is added to formalin and is stirred by magneton, triethanolamine is then added and adjusts mixture pH It is stirred to react after value, is after reaction cooled to room temperature mixture and is diluted with deionized water.
Wherein, the dosage of the urea and formalin is 12g:24.5g;Wherein, formalin concentration is 37 wt%;
It is 8-10 that the addition triethanolamine, which adjusts mixture pH,;
Described be stirred to react is stirred to react 1-1.5h for 70 DEG C.
(3) preparation of hydrophily macropore ureaformaldehyde adsorbent (UFMF)
Firstly, under mechanical stirring, in the round-bottomed flask that ureaformaldehyde monomer and lignin dispersion liquid are added to;In stirring bar Toluene is slowly added dropwise under part and into water phase as organic phase;Stirring is formed uniform after toluene adjusts revolving speed after being added dropwise completely Pik woods High Internal Phase Emulsion template;The lotion of formation is transferred in centrifuge tube, product is obtained after polymerization reaction;Then with ethyl alcohol Washing purifying is carried out to product for the eluant, eluent of Soxhlet extraction, to remove unreacted monomer and remaining organic solvent;Finally, Keep product UFMF dry.
Wherein, the volume ratio of the ureaformaldehyde monomer and lignin dispersion liquid is 1.0:0.1-1.0;
The speed of agitator is 600 rpm-900rpm;
The volume ratio of the ureaformaldehyde monomer and toluene is 1.0:3-5;
Revolving speed is adjusted to 1000rpm after the toluene is added dropwise completely, stirs 1.0-1.5h;
The polymerization reaction is to polymerize 24 h at 65 DEG C -75 DEG C;
The drying condition is dry 24 h at 25 DEG C -40 DEG C.
Hydrophily macropore ureaformaldehyde adsorbent prepared by the present invention is shelly-shaped urea formaldehyde polymer material, and cellular structure can pass through Control lotion grease Phase Proportion and polymerization time and change, density is small, light weight.
Beneficial effects of the present invention:
Exhibiting high surface activating agent be will use in the preparation process of traditional High Internal Phase Emulsion to cause to endanger to environment and human body Evil, the stable particle of common pickering emulsion often need chemical modification, to ensure that it is steady that the surface wettability of stable particle is enough to obtain Fixed emulsion system, it is modified and resourceful that the biological material lignin that the present invention uses does not need surface, through a step lotion It can be obtained stable O/W type pickering emulsion, method is simple, low in cost.In addition, macrocellular foam type produced by the present invention is inhaled Attached dose of presoma is the monomer of formaldehyde and urea polycondensation, and raw material is simple, low in cost, and is had using it as the adsorbent of monomer preparation The functional groups such as amino abundant, carbonyl, can be used as and be effectively combined site.
Macrocellular foam type adsorbent permeability produced by the present invention is good, porosity is high, permeability is good, and macroporous structure can add Strong pollutant is diffused into adsorption site through liquid medium, improves mass-transfer efficiency;Its cellular structure can be by controlling lotion grease Phase Proportion and polymerization time and change, to cope with the absorption under different condition;The macrocellular foam type adsorbent density obtained simultaneously Small, light weight, therefore the adsorption potential points of unit mass are much higher than solid adsorbent.In addition, the adsorbent surface hydrophily is very It is good, can ensure that adsorbent dispersion stable in water solution system, this feature for absorbing phenolic etc. can in water slightly soluble, can Molten organic matter is advantageous, therefore is well suited for the adsorbing separation of organic pollutant in environment water solution system.
Detailed description of the invention
Fig. 1 is to be comparably 75% (a) in pik woods High Internal Phase Emulsion, optical microscopy when 80 (b), 85% (c) Figure;Scale is 10 μm in figure.
Fig. 2 is that in a large amount of water (a) and (b) in toluene is added dropwise in preparation O/W type pik woods High Internal Phase Emulsion in embodiment 1 Result figure.
Fig. 3 is the UFMF scanning electron microscope (SEM) photograph (a) prepared in embodiment 1 and the UFMF scanning after adsorption-desorption recycles Electron microscope (b).
Fig. 4 is the lignin (a) prepared in embodiment 1 and the infrared spectrogram of UFMF (b).
Fig. 5 is the lignin (a) prepared in embodiment 1 and the contact angle of UFMF (b).
Fig. 6 is the lignin (a) prepared in embodiment 1 and the thermogravimetric analysis figure of UFMF (b).
Specific embodiment
Recognition performance evaluation carries out by the following method in the specific embodiment of the invention: complete using Staticadsorption experiment At.By 10mL certain density 2,4,5-TCP, 2,4,6TCP and 4-NP solution is added in centrifuge tube, and a certain amount of parent is added Aqueous ureaformaldehyde macroporous adsorbent UFMF is placed in 25 DEG C of constant temperature waters and stands several hours, 2,4,5-TCP, 2,4,6- after absorption TCP and 4-NP content is measured with ultraviolet-uisible spectrophotometer, and calculates adsorption capacity according to result.
Below with reference to specific implementation example, the present invention will be further described.
Embodiment 1:
(1) preparation of lignin dispersion liquid:
The lignin of 7.5 g is added to the lignin dispersion that 7.5 % of mass fraction is formed in 92.5 mL deionized waters Liquid, to ensure that lignin can disperse completely, the pH value of mixture to be adjusted by the way that concentrated ammonia liquor (volume content 25%) is added dropwise, until pH Value is 11.Then said mixture is filtered to remove impurity.Make lignin finally, hydrochloric acid (1 M) is added dropwise in filtrate and adjusts pH to 3 Dispersion stable is with spare.
(2) preparation of ureaformaldehyde (UF) monomer:
Firstly, 12 g urea are added to the 37 wt% formalins of 24.5 g and are stirred by magneton, it is then added three Ethanol amine adjusts mixture ph and is stirred to react 1.0h to 8.5,70 DEG C, is cooled to room temperature mixture is used in combination after reaction The dilution of 50mL deionized water.
(3) preparation of hydrophily macropore ureaformaldehyde adsorbent (UFMF):
Firstly, under mechanical stirring, by 5.4 mL ureaformaldehyde monomers and 0.6 mL lignin dispersion liquid (7.5 % of mass fraction) It is added in the round-bottomed flask of 100 mL.Stirring under 600 rpm revolving speeds and 24 mL toluene are slowly added dropwise into water phase and are used as has Machine phase.Revolving speed is adjusted to 1000 rpm to stir 1.0 hours by toluene after being added dropwise completely forms uniform pik woods High Internal Phase Emulsion Template.The lotion of formation is transferred in centrifuge tube, 24 h are polymerize at 70 DEG C and obtain product.Then it is mentioned by Soxhlet of ethyl alcohol The eluant, eluent taken carries out washing purifying to product, to remove unreacted monomer and remaining organic solvent.Finally, at 25 DEG C Make dry 24 h of product UFMF at room temperature.
Fig. 2 is to prepare O/W type pik woods High Internal Phase Emulsion in embodiment 1 in a large amount of water (a) and (b) in toluene is added dropwise Result figure.(a) is schemed it can be seen that disintegration, figure (b) emulsion droplet are still able to maintain surely in toluene immediately after lotion instills in water It is fixed, show successfully to prepare stable O/W type High Internal Phase Emulsion.
Fig. 3 is the UFMF scanning electron microscope (SEM) photograph (a) prepared in embodiment 1, and UFMF as shown in the figure contains a large amount of macropore and company Hole is connect, size distribution is relatively narrow, relatively uniform;Scheming (b) is the UFMF scanning electron microscope (SEM) photograph after adsorption-desorption recycles, material Material pattern, which is not substantially change, shows it with preferable stability.
Fig. 4 is the lignin (a) prepared in embodiment 1 and the infrared spectrogram of UFMF (b);Show successfully to prepare shelly-shaped Urea formaldehyde polymer material.
Fig. 5 is the lignin (a) prepared in embodiment 1 and the contact angle of UFMF (b);It can be seen that lignin itself has Good surface wettability is to stablize O/W type lotion;The UFMF material surface of preparation shows very strong hydrophily.
Fig. 6 is the lignin (a) prepared in embodiment 1 and the thermogravimetric analysis figure of UFMF (b);When in start temperature ranges (< 250 DEG C), UFMF and lignin weight loss substantially 10.52% and 7.15%, predominantly physics absorbs water at this time, shows that UFMF has There is good hydrophily;When temperature is increased to 800 DEG C, the obvious weight loss that material occurs is UFMF thermal decomposition amount, is also indicated that Material has good thermal stability.
Embodiment 2:
(1) preparation of lignin dispersion liquid:
The lignin of 3.0 g is added to the lignin dispersion liquid that 3.0 % of mass fraction is formed in 97 mL deionized waters, To ensure that lignin can disperse completely, the pH value of mixture to be adjusted by the way that concentrated ammonia liquor (volume content 25%) is added dropwise, until pH value is 9.Then said mixture is filtered to remove impurity.Disperse lignin finally, hydrochloric acid (1 M) is added dropwise in filtrate and adjusts pH to 5 Liquid is stablized with spare.
(2) preparation of ureaformaldehyde (UF) monomer:
Firstly, 12 g urea are added to the 37 wt% formalins of 24.5 g and are stirred by magneton, it is then added three Ethanol amine adjusts mixture ph and is stirred to react 1.5h to 10,70 DEG C, is cooled to room temperature mixture is used in combination after reaction The dilution of 50mL deionized water.
(3) preparation of hydrophily macropore ureaformaldehyde adsorbent (UFMF):
Firstly, under mechanical stirring, 5 mL ureaformaldehyde monomers and 5 mL lignin dispersion liquids (3.0 % of mass fraction) are added Into the round-bottomed flask of 100 mL.It is stirred under 900 rpm revolving speeds and 20 mL toluene is slowly added dropwise into water phase as organic Phase.Revolving speed is adjusted to 1000 rpm to stir 1.5 hours by toluene after being added dropwise completely forms uniform pik woods High Internal Phase Emulsion mould Plate.The lotion of formation is transferred in centrifuge tube, 24 h are polymerize at 75 DEG C and obtain product.Then using ethyl alcohol as Soxhlet extraction Eluant, eluent washing purifying is carried out to product, to remove unreacted monomer and remaining organic solvent.Finally, at 40 DEG C Make dry 24 h of product UFMF.
Embodiment 3:
(1) preparation of lignin dispersion liquid:
The lignin of 5.0 g is added to the lignin dispersion that 5.0 % of mass fraction is formed in 95.0 mL deionized waters Liquid, to ensure that lignin can disperse completely, the pH value of mixture to be adjusted by the way that concentrated ammonia liquor (volume content 25%) is added dropwise, until pH Value is 10.Then said mixture is filtered to remove impurity.Make lignin finally, hydrochloric acid (1 M) is added dropwise in filtrate and adjusts pH to 4 Dispersion stable is with spare.
(2) preparation of ureaformaldehyde (UF) monomer:
Firstly, 12 g urea are added to the 37 wt% formalins of 24.5 g and are stirred by magneton, it is then added three Ethanol amine adjusts mixture ph and is stirred to react 1 h to 8,70 DEG C, is after reaction cooled to room temperature mixture and uses 50mL Deionized water dilution.
(3) preparation of hydrophily macropore ureaformaldehyde adsorbent (UFMF):
Firstly, under mechanical stirring, by 4.8 mL ureaformaldehyde monomers and 1.2 mL lignin dispersion liquids (5.0 % of mass fraction) It is added in the round-bottomed flask of 100 mL.Stirring under 800 rpm revolving speeds and 24 mL toluene are slowly added dropwise into water phase and are used as has Machine phase.Revolving speed is adjusted to 1000 rpm to stir 1.5 hours by toluene after being added dropwise completely forms uniform pik woods High Internal Phase Emulsion Template.The lotion of formation is transferred in centrifuge tube, 24 h are polymerize at 70 DEG C and obtain product.Then it is mentioned by Soxhlet of ethyl alcohol The eluant, eluent taken carries out washing purifying to product, to remove unreacted monomer and remaining organic solvent.Finally, at 30 DEG C Under make dry 24 h of product UFMF.
Fig. 1 is to be comparably 75% (a) in pik woods High Internal Phase Emulsion, optical microscopy when 80 (b), 85% (c) Figure;Scale is 10 μm in figure.The lotion of formation is played very as shown, lignin can be located at oil-water two-phase interfaces Good stabilization;With the interior raising compared, more crowded and drop average diameter is also reduced between emulsion droplet.
The absorption property of material prepared by the present invention is proved below by test example.
Test example 1: respectively taking 10mL initial concentration is 2,4,5-TCP, 2,4,6-TCP and 10mL initial concentration of 100mg/L It is added separately in centrifuge tube for the 4-NP of 50mg/L, then the hydrophily ureaformaldehyde macroporous absorption being separately added into 10mg embodiment 1 Agent (UFMF), is placed on test fluid in 25 DEG C of water bath chader, respectively 5.0,15,30,60,120,240,360,480, It is taken out when 720 min;Adsorbent and solution are separated by being centrifuged, it is fine to reuse the micropore nitric acid that aperture is 0.45mm It ties up plain film and the particle that removal suspends is filtered to solution.2,4,5-TCP, 2,4,6-TCP and 4-NP in filtrate is by ultraviolet point Light photometer 292nm, 288 nm, 252 nm wavelength under or Atomic absorption calculate measurement, and absorption is calculated according to result Capacity;The result shows that 2,4,5-TCP adsorption capacity quicklys increase in initial 25min, this is the result shows that 2,4,5-TCP It is better than 2,4,6-TCP and 4-NP in UFMF diffusion into the surface rate;In addition, UFMF to 2,4,5-TCP adsorption capacity also than 2,4, 6-TCP and 4-NP is big;After quick adsorption, the rate of adsorption sharply declines and reaches balance in 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) are added in centrifuge tube, while taking the 10mL initial concentration to be respectively respectively 10, the 4-nitrophenols (4-NP) of 20,30,40,50 mg/L and the respectively parent into three groups of centrifuge tubes addition 10mg embodiments 1 Aqueous ureaformaldehyde macroporous adsorbent (UFMF), is placed on test fluid after standing for 24 hours in 25 DEG C of water-bath, supernatant liquor high speed centrifugation Machine separates and collects, unadsorbed 2,4,5-TCP, 2,4,6-TCP and 4-NP by ultraviolet specrophotometer 292nm, 288 nm, Under the wavelength of 252 nm or Atomic absorption calculates measurement, and calculates adsorption capacity according to result, the results showed that, it is flat to reach absorption When weighing apparatus the maximum adsorption capacity of 2,4,5-TCP, 2,4,6-TCP and 4-NP be respectively 116.3 μm of ol/g, 78.74 μm of ol/g and In comparison more preferably, the type for showing substituent group and position are simultaneously for the effect of 29.4 μm of ol/g, UFMF absorption 2,4,5-TCP Having an impact to adsorption effect and showing as 2,4,5- chlorine replaces position > 2,4,6- chlorine that position > 4- nitro is replaced to replace position.

Claims (8)

1. a kind of macropore ureaformaldehyde adsorbent, which is characterized in that the adsorbent cellular structure can be compared by controlling lotion grease Example and polymerization time and change, containing a large amount of macropore and connecting hole, the adsorbent follows the steps below preparation:
(1) preparation of lignin dispersion liquid:
Lignin is add to deionized water and prepares lignin dispersion liquid, the pH value that concentrated ammonia liquor adjusts mixture is added dropwise;Then Mixture is filtered to remove impurity;Make lignin dispersion stable with spare finally, salt acid for adjusting pH is added dropwise in filtrate;
(2) preparation of ureaformaldehyde (UF) monomer:
Urea is added to formalin and is stirred by magneton, it is anti-that stirring after triethanolamine adjusts mixture ph is then added It answers, be after reaction cooled to room temperature mixture and diluted with deionized water;
(3) preparation of hydrophily macropore ureaformaldehyde adsorbent (UFMF):
Firstly, under mechanical stirring, ureaformaldehyde monomer and lignin dispersion liquid are added in round-bottomed flask;Under agitation simultaneously Toluene is slowly added dropwise into water phase as organic phase;Stirring forms uniform pik woods after toluene adjusts revolving speed after being added dropwise completely High Internal Phase Emulsion template;The lotion of formation is transferred in centrifuge tube, product is obtained after polymerization reaction;Then using ethyl alcohol as Soxhlet The eluant, eluent of extraction carries out washing purifying to product, to remove unreacted monomer and remaining organic solvent;Finally, making product UFMF is dry;
The dosage of urea described in step (2) and formalin is 12g:24.5g;Wherein, formalin concentration is 37 wt%;
The volume ratio of ureaformaldehyde monomer described in step (3) and lignin dispersion liquid is 1.0:0.1-1.0;
Polymerization reaction described in step (3) is to polymerize 24 h at 65 DEG C -75 DEG C.
2. a kind of macropore ureaformaldehyde adsorbent according to claim 1, which is characterized in that lignin as described in step (1) The concentration of dispersion liquid is 3.0-7.5 wt%;The pH value of the mixture is 9-11;
The pH that lignin dispersion liquid is adjusted after the dropwise addition hydrochloric acid is 3-5;Wherein concentration of hydrochloric acid is 1M.
3. a kind of macropore ureaformaldehyde adsorbent according to claim 1, which is characterized in that the addition triethanolamine adjusts mixed Conjunction object pH is 8-10;
Described be stirred to react is stirred to react 1-1.5h for 70 DEG C.
4. a kind of macropore ureaformaldehyde adsorbent according to claim 1, which is characterized in that speed of agitator described in step (3) For 600 rpm-900rpm;The volume ratio of the ureaformaldehyde monomer and toluene is 1.0:3-5.
5. a kind of macropore ureaformaldehyde adsorbent according to claim 1, which is characterized in that toluene described in step (3) is added dropwise Revolving speed is adjusted to 1000rpm after completely, stirs 1.0-1.5h.
6. a kind of macropore ureaformaldehyde adsorbent according to claim 1, which is characterized in that drying condition described in step (3) It is dry 24 h at 25 DEG C -40 DEG C.
7. macropore ureaformaldehyde adsorbent described in claim 1 in aqueous solution phenolic comp ' ds pollution absorption and isolated application.
8. application according to claim 7, which is characterized in that the phenolic comp ' ds pollution be 2,4,5- trichlorophenol, 2,4,6,-Ts, 2,4, 6- trichlorophenol, 2,4,6,-T, 4-nitrophenols.
CN201610659545.2A 2016-08-12 2016-08-12 A kind of method of emulsion template method preparation hydrophily macropore ureaformaldehyde adsorbent Expired - Fee Related CN106268686B (en)

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