CN105195101A - Preparation method of beta-cyclodextrin modified nanometer silicon nitride adsorbent - Google Patents
Preparation method of beta-cyclodextrin modified nanometer silicon nitride adsorbent Download PDFInfo
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Abstract
The invention discloses a preparation method of a beta-cyclodextrin modified nanometer silicon nitride adsorbent. The method comprises the steps that silicon nitride is pretreated in a dimethyl sulfoxide and anhydrous ethanol solvent through gamma-isocyanate propyl triethoxy silane; then in a reactor, by mass, 55-65% of N,N-dimethylformamide and 7-17% of beta-cyclodextrin are added and are stirred and dissolved, then the temperature is increased to 55+/-2 DEG C and kept constant, stirring is carried out, a backflow reaction is carried out for 4.5-6.5 h, 20-30% of pretreated silicon nitride is added, the sum of the percentages of all the components is 100%, the constant temperature is kept at 90+/-2 DEG C, stirring is carried out, the backflow reaction is carried out for 8-10 h, acetone backflow washing is carried out after the reaction is finished, the mixture is taken out to be placed in a vacuum drying box to be dried, and the beta-cyclodextrin modified nanometer silicon nitride adsorbent is obtained. The beta-cyclodextrin modified nanometer silicon nitride adsorbent has the high adsorption capacity for bisphenol A, can be repeatedly used, and is low in cost and resistant to high temperature.
Description
Technical field
The present invention relates to the technical field of a kind of preparation method of adsorbent, particularly a kind of preparation method of beta-schardinger dextrin-modified Nano silicon nitride adsorbent and application technology that bisphenol-A (BPA) is adsorbed.
Background technology
Nano-silicon nitride is a kind of superhard material, and itself has lubricity, and wear-resistant, is atomic crystal; Anti-oxidant during high temperature.And it can also resist thermal shock, be heated to more than 1000 DEG C in atmosphere, quick refrigeration sharply heats again, also can not be cracked.In a broad sense, nano material refers to the material having at least one dimension to be in nanoscale scope (0.1nm ~ 100nm) or to be made up of as elementary cell them in three dimensions.Nano material has following four features: (1) surface and interface effect: this refers to that the ratio of nanocrystal grain surface atom number and total atom number diminishes with particle diameter and sharply increases rear caused qualitative change.Such as, when particle diameter is 10 nanometer, particulate comprises 4000 atoms, and surface atom accounts for 40%; When particle diameter is 1 nanometer, particulate includes 30 atoms, and surface atom accounts for 99%.Main cause is just that diameter reduces, surface atom increasing number.(2) small-size effect: when nanoparticle size and optical wavelength, the physical features sizes such as the de Broglie wavelength of conduction electron and the coherence length of superconducting state, transmission depth quite or less time, its periodic boundary is destroyed, thus making its sound, optical, electrical, magnetic, the performances such as thermodynamics present the phenomenon of " novelty ".(3) quantum size effect: when the size of particle reaches nanometer scale, the electron energy level near fermi level splits into discrete energy levels by continuous state.When energy level spacing is greater than the cohesion energy of heat energy, magnetic energy, electrostatic energy, magnetostatic energy, photon energy or superconducting state, there will be the quantum effect of nano material, thus make its magnetic, light, sound, heat, electricity, superconduct performance change.(4) macro quanta tunnel effect: microcosmic particle has the ability running through potential barrier and is called tunnel-effect.The intensity of magnetization of nano particle etc. also have tunnel-effect, and they can change through the potential barrier of macrosystem, this macro quanta tunnel effect being called as nano particle.Due to nano-silicon nitride special nature, using nano-silicon nitride to have as the skeleton of adsorbent, to connect site many, stable chemical nature, applied range.
Beta-schardinger dextrin-is a series of with the cyclic oligosaccharide of α-Isosorbide-5-Nitrae-glycoside link, in truncated cones shape Kranz structure, has interior hydrophobic and outer hydrophily, and the molecule suitable to size can carry out bag and connect.This special character makes it be widely applied in pharmaceutical carrier, chiral Recognition, Chemical Decomposition, electrochemical sensing etc.In recent years, many scholars start to pay close attention to beta-schardinger dextrin-and the application of derivative in environmental area thereof.Sun Linlin etc., have studied carboxymethyl-beta-cyclodextrin functionalization ferroferric oxide magnetic nano compound to the absorption property (Sun Linlin etc. of rhodamine B, carboxymethyl-beta-cyclodextrin functionalization ferroferric oxide magnetic nano compound is to the absorption property of rhodamine B, applied chemistry, 2015,32(1): 110-117); Li Wei etc. have studied preparation and the absorption property (Li Wei etc., the preparation of beta-cyclodextrin modified polyvinyl alcohol nano and Study on adsorption properties thereof, 2013,20(4) thereof of beta-cyclodextrin modified polyvinyl alcohol nano: 21-24).
In recent years, in water environment, the appearance of endocrine disruptor causes the extensive concern of people.Bisphenol-A (BPA) is widely used in produces synthetic resin, plastics, synthetic fibers and agricultural chemicals.Meanwhile, BPA is again important environment incretion interferent, it can with the endogenous hormones estradiol competition binding ERs of human body, and a series of pathology may be caused, Long Term Contact BPA can increase suffer from a heart complaint, the risk of diabetes and hepatopathy.Product containing BPA in use can entered environment thus harm humans is healthy by all means, and if baby bottles is in Long Term Contact comparatively hot liquid, BPA can discharge gradually thus produce potential hazard to the brain of immunoenzyme technics, behavior and prostate.Therefore, on October 18th, 2008, federal government of Canada announced, determined BPA to list in noxious material list.Therefore, to the waste water in drinking water in life and industrial production except BPA, being the important topic being related to the people's livelihood, is also the focus of domestic and international experts and scholars research.
When entering society, water pollution problems causes people more and more to pay close attention to.Along with day by day increasing the weight of of water pollution problems, prepare with strong points, treatment effect good, the new material that can reuse becomes research emphasis.
The organic and inorganic pollutant that exists in adsorbing separation removing ambient water, has been considered to a kind of very effective and conventional processing method, and employing adsorption method of separation becomes those skilled in the art's concerned issue except the BPA in anhydrating.Adopt adsorbing separation removing BPA to have reported, Liu Guifang etc. have studied the absorption (Liu Guifang etc., the absorption research of bisphenol-A in Aqueous Solution on Modified Activated Carbons, environmental science, 2008,29(2) of bisphenol-A in Aqueous Solution on Modified Activated Carbons: 349-355); Woods Fu Hua etc. have studied the application (Lin Fuhua etc. of sorption extraction stirring rod in environmental water sample content of bisphenol A measures that molecularly imprinted polymer is coating; molecularly imprinted polymer is the application of sorption extraction stirring rod in environmental water sample content of bisphenol A measures of coating; chromatogram; 2010,28(5): 507-512) disclose redox graphene-Fe in Chinese patent CN103418340A
3o
4the application of nano composite material and preparation method thereof and absorption bisphenol-A; Preparation method and the application of bisphenol-A in adsorption treatment water body thereof of the U.S. aluminum binary houghite of a kind of modification is disclosed in Chinese patent CN102167371B.
Summary of the invention
An object of the present invention is to provide a kind of preparation method of beta-schardinger dextrin-modified Nano silicon nitride adsorbent, and a kind of beta-schardinger dextrin-modified Nano silicon nitride adsorbent of acquisition carries out adsorbing separation to BPA in aqueous systems.
Object of the present invention is achieved through the following technical solutions.
A preparation method for beta-schardinger dextrin-modified Nano silicon nitride adsorbent, is characterised in that the method has following processing step:
(1) silicon nitride pretreatment: in the reactor, adds by by following composition mass percent, methyl-sulfoxide: 15 ~ 25%, absolute ethyl alcohol: 35 ~ 45%, γ-isocyanatopropyl triethoxysilane: 10 ~ 20%, stirs, mix, then add as nano-silicon nitride: 20 ~ 30%, each component sum is absolutely, in 90 ~ 95 DEG C of constant temperature, stirring, back flow reaction 6 ~ 8h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, drying, obtains pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add by following composition mass percent, N, dinethylformamide: 55 ~ 65%, beta-schardinger dextrin-: 7 ~ 17%, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stir, back flow reaction 4.5 ~ 6.5h, add pretreatment silicon nitride again: 20 ~ 30%, each component sum is absolutely, in 90 ± 2 DEG C of constant temperature, stir, back flow reaction 8 ~ 10h, wash with acetone reflux after completion of the reaction, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
The particle diameter of described silicon nitride is between 50 ~ 100nm.
Methyl-sulfoxide described in step (1) and absolute ethyl alcohol volume ratio are optimum in the scope of 1:1.5 ~ 2.
Beta-schardinger dextrin-described in step (2) and pretreatment silicon nitride mass ratio are optimum in the scope of 1:3 ~ 4.
Another object of the present invention be to provide a kind of beta-schardinger dextrin-modified Nano silicon nitride adsorbent in aqueous systems to the absorption of BPA, feature is: the beta-schardinger dextrin-modified Nano silicon nitride adsorbent deionized water for preparing is soaked 2 ~ 3h, adsorbs by static method.
The beta-schardinger dextrin-modified Nano silicon nitride adsorbent deionized water prepared is soaked 2 ~ 3h, adsorbs by dynamic method.
Compared with the prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the beta-schardinger dextrin-modified Nano silicon nitride adsorbent that the present invention obtains has good physical and chemical stability and excellent mechanical strength, adsorption capacity is large, maximum adsorption capacity reaches 132.12mg/g, wear-resistingly can reach more than 15 times by Reusability number of times, the speed of absorption is fast, and absorption chooses, and desorption performance is good, can use within the scope of wider soda acid, the carrier property making adsorbent than silica is superior.
(2) the beta-schardinger dextrin-modified Nano silicon nitride that the present invention obtains both had had the advantage of solid support material, also solved active group beta-schardinger dextrin-and was applied to losing issue in water environment.
(3) condition of the process entails synthesized easily controls, and energy consumption is low, simple to operate, belongs to process for cleanly preparing, is easy to suitability for industrialized production.
Detailed description of the invention
Embodiment 1
(1) silicon nitride pretreatment: in the reactor, adds respectively, methyl-sulfoxide: 18mL, absolute ethyl alcohol: 45mL, γ-isocyanatopropyl triethoxysilane: 15mL, stirs, mix, add again as nano-silicon nitride: 25g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 7h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, dry, obtain pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add respectively, DMF: 63mL, beta-schardinger dextrin-: 13g, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stirring, back flow reaction 5h, then add pretreatment silicon nitride: 27g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 9h, after completion of the reaction with acetone reflux washing, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
Embodiment 2
(1) silicon nitride pretreatment: in the reactor, adds respectively, methyl-sulfoxide: 14mL, absolute ethyl alcohol: 50mL, γ-isocyanatopropyl triethoxysilane: 10mL, stirs, mix, add again as nano-silicon nitride: 30g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, dry, obtain pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add respectively, DMF: 68mL, beta-schardinger dextrin-: 7g, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stirring, back flow reaction 4.5h, then add pretreatment silicon nitride: 28g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 8h, after completion of the reaction with acetone reflux washing, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
Embodiment 3
(1) silicon nitride pretreatment: in the reactor, adds respectively, methyl-sulfoxide: 23mL, absolute ethyl alcohol: 39mL, γ-isocyanatopropyl triethoxysilane: 20mL, stirs, mix, add again as nano-silicon nitride: 20g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 8h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, dry, obtain pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add respectively, DMF: 58mL, beta-schardinger dextrin-: 15g, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stirring, back flow reaction 5.5h, then add pretreatment silicon nitride: 30g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 10h, after completion of the reaction with acetone reflux washing, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
Embodiment 4
(1) silicon nitride pretreatment: in the reactor, adds respectively, methyl-sulfoxide: 17mL, absolute ethyl alcohol: 47mL, γ-isocyanatopropyl triethoxysilane: 18mL, stirs, mix, add again as nano-silicon nitride: 22g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 6.5h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, dry, obtain pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add respectively, DMF: 72mL, beta-schardinger dextrin-: 12g, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stirring, back flow reaction 6h, then add pretreatment silicon nitride: 20g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 8.5h, after completion of the reaction with acetone reflux washing, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
Embodiment 5
(1) silicon nitride pretreatment: in the reactor, adds respectively, methyl-sulfoxide: 20mL, absolute ethyl alcohol: 43mL, γ-isocyanatopropyl triethoxysilane: 12mL, stirs, mix, add again as nano-silicon nitride: 28g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 7.5h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, dry, obtain pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add respectively, DMF: 67mL, beta-schardinger dextrin-: 10g, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stirring, back flow reaction 6.5h, then add pretreatment silicon nitride: 26g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 9.5h, after completion of the reaction with acetone reflux washing, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
Embodiment 6
(1) silicon nitride pretreatment: in the reactor, adds respectively, methyl-sulfoxide: 10mL, absolute ethyl alcohol: 24mL, γ-isocyanatopropyl triethoxysilane: 8mL, stirs, mix, add again as nano-silicon nitride: 13g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 7h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, dry, obtain pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add respectively, DMF: 30mL, beta-schardinger dextrin-: 6g, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stirring, back flow reaction 5h, then add pretreatment silicon nitride: 14g, in 90 ± 2 DEG C of constant temperature, stirring, back flow reaction 9h, after completion of the reaction with acetone reflux washing, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
Embodiment 7
Take 0.20g beta-schardinger dextrin-modified Nano silicon nitride adsorbent and be placed in 250mL tool plug conical flask immersion 2 ~ 3h, after filtration washing, adding 100mL concentration is in 400mg/LBPA standard liquid, be in 2.0 ~ 9.0 scopes with the pH value of diluted acid or alkali regulation system, at room temperature shake absorption 1 ~ 4h, get supernatant, electrochemically measure the concentration of BPA, according to the concentration difference of BPA in water before and after absorption, calculate the adsorption capacity of beta-schardinger dextrin-modified Nano silicon nitride adsorbent, beta-schardinger dextrin-modified Nano silicon nitride adsorbent obtained by the present invention is maximum and stable to the absorption pH value of BPA adsorbent adsorption capacity to BPA in 6.0 ~ 7.0 scopes, at room temperature concussion absorption 1.5h, BPA adsorbs completely substantially, the adsorption capacity of BPA can reach 132.12mg/g.
Embodiment 7
Take 1.0g beta-schardinger dextrin-modified Nano silicon nitride adsorbent and be placed in 250mL tool plug conical flask immersion 2 ~ 3h, after filtration washing, adding 100mL concentration is in 200mg/LBPA standard liquid, be in 6.0 ~ 7.0 scopes with the pH value of diluted acid or alkali regulation system, at room temperature concussion absorption 2h, get supernatant, electrochemically measure the concentration of BPA, according to the concentration difference of BPA in water before and after absorption, calculate beta-schardinger dextrin-modified Nano silicon nitride adsorbent to the clearance of BPA, beta-schardinger dextrin-modified Nano silicon nitride adsorbent obtained by the present invention to the clearance of BPA all more than 95.62%, reach as high as 99%.
Claims (5)
1. a preparation method for beta-schardinger dextrin-modified Nano silicon nitride adsorbent, is characterized in that, the method has following processing step:
(1) silicon nitride pretreatment: in the reactor, adds by by following composition mass percent, methyl-sulfoxide: 15 ~ 25%, absolute ethyl alcohol: 35 ~ 45%, γ-isocyanatopropyl triethoxysilane: 10 ~ 20%, stirs, mix, then add as nano-silicon nitride: 20 ~ 30%, each component sum is absolutely, in 90 ~ 95 DEG C of constant temperature, stirring, back flow reaction 6 ~ 8h, be cooled to room temperature after completion of the reaction, with absolute ethanol washing, filter, drying, obtains pretreatment silicon nitride;
(2) beta-schardinger dextrin-modified Nano silicon nitride absorbent preparation: in the reactor, add by following composition mass percent, N, dinethylformamide: 55 ~ 65%, beta-schardinger dextrin-: 7 ~ 17%, after stirring and dissolving, be warming up to 55 ± 2 DEG C of constant temperature, stir, back flow reaction 4.5 ~ 6.5h, add pretreatment silicon nitride again: 20 ~ 30%, each component sum is absolutely, in 90 ± 2 DEG C of constant temperature, stir, back flow reaction 8 ~ 10h, wash with acetone reflux after completion of the reaction, put in vacuum drying chamber dry after taking-up, obtain beta-schardinger dextrin-modified Nano silicon nitride adsorbent.
2., according to the preparation method of a kind of beta-schardinger dextrin-modified Nano silicon nitride adsorbent described in claim 1, it is characterized in that, the particle diameter of the silicon nitride described in step (1) is between 50 ~ 100nm.
3. according to the preparation method of a kind of beta-schardinger dextrin-modified Nano silicon nitride adsorbent described in claim 1, it is characterized in that, the methyl-sulfoxide described in step (1) and absolute ethyl alcohol volume ratio are optimum in the scope of 1:1.5 ~ 2.
4. according to the preparation method of a kind of beta-schardinger dextrin-modified Nano silicon nitride adsorbent described in claim 1, it is characterized in that, the beta-schardinger dextrin-described in step (2) and pretreatment silicon nitride mass ratio are optimum in the scope of 1:3 ~ 4.
5. the beta-schardinger dextrin-modified Nano silicon nitride adsorbent prepared by the preparation method of a kind of beta-schardinger dextrin-modified Nano silicon nitride adsorbent described in claim 1.
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