CN104722265A - Preparation method and application of modified attapulgite adsorbent - Google Patents
Preparation method and application of modified attapulgite adsorbent Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a modified attapulgite adsorbent, and belongs to the technical field of pollution control of a water body. The preparation method comprises the following steps: firstly, carrying out acidification on attapulgite by adopting a hydrochloric acid solution; carrying out amination treatment on the acidified attapulgite; and modifying the attapulgite by ethylenediamine tetraacetic acid to prepare the modified attapulgite adsorbent. The method for preparing the modified attapulgite adsorbent from the attapulgite modified by ethylenediamine tetraacetic acid is simple to operate and has low requirements on equipment; the attapulgite is readily available and the price is low; and the prepared modified attapulgite adsorbent has a good adsorption performance. The modified attapulgite adsorbent prepared by the preparation method can be effectively applied to trivalent chromium treatment of industrial wastewater.
Description
Technical field
The invention belongs to water pollution control technical field, be specifically related to a kind of preparation method and application thereof of modified attapulgite earth adsorbing.
Background technology
Along with socioeconomic development, the discharge of industrial wastewater becomes a large problem of environment aspect, the pollution of heavy metal in waste water is particularly serious, especially pollution of chromium, pollution of chromium is trivalent chromium and chromic harm mainly, although chromic toxicity does not have chromic strong toxicity, it can not be ignored the health of environment and human body.
Have a lot for chromic minimizing technology at present, such as electrolysis, membrane separation process, absorption method etc., in the chromic method of numerous removal, absorption method is a kind of simple to operate, method for treating water efficiently and effectively, adsorbent can utilize the loose structure of itself to hold heavy metal ion, or by contained various active group itself as hydroxyl, carboxyl, amino etc., form ionic bond or covalent bond with metal ion, reach the object of removal metal ion.
Attapulgite be a kind of have chain layer structure containing Shuifu County's zeopan clay mineral, become tiny bar-shaped, there is larger specific area and more duct.In China, attapulgite rich reserves, price is comparatively cheap.Due to attapulgite itself have that specific area is large, the feature such as absorption property is strong, source is wide and cost is low, therefore may be used for sewage disposal.
Because attapulgite has certain removal effect to trivalent chromium in water, but adsorbance is lower, therefore, be necessary to carry out modification to attapulgite, as adopted polyaniline, γ-aminopropylsilane, shitosan etc. carry out modification to attapulgite, and use it for chromic removal in water.Along with these adsorbents have certain removal effect to trivalent chromium in water, but when there is organic complex in absorption system, this type of adsorbent greatly can be reduced to removal effect chromic in water.
Summary of the invention
The object of the present invention is to provide a kind of preparation method and application thereof of modified attapulgite earth adsorbing, this preparation method is simple to operate, low for equipment requirements; The wide material sources of attapulgite, cheap, obtained attapulgite modified adsorbent performance is good.
The present invention is achieved through the following technical solutions:
A preparation method for modified attapulgite earth adsorbing, comprises the following steps:
1) attapulgite is added in hydrochloric acid solution, ultrasonic disperse, then react at 60 ~ 80 DEG C, cross leaching precipitation, by washing of precipitate to neutral, dry, the attapulgite of obtained acidifying;
2) attapulgite of acidifying is added in toluene, ultrasonic disperse, obtain mixed solution; Then under nitrogen protection, by mixed solution by room temperature to 110 ~ 120 DEG C, add aminopropyl trimethoxysilane, continue to stir, filter, get precipitation, after solid extracting, vacuum drying, obtained composite nano materials;
3) under nitrogen protection, get carrene and ethylenediamine tetra-acetic acid, drip thionyl chloride under constant voltage, then add step 2) obtained composite nano materials, after reacting 2 ~ 3h under room temperature, cross leaching precipitation; By dry after washing of precipitate, obtained modified attapulgite earth adsorbing.
Step 1) be in 1g:(15 ~ 25) ratio of mL, attapulgite is added in the hydrochloric acid solution of 1 ~ 5mol/L, ultrasonic disperse 10 ~ 20min, then at 60 ~ 80 DEG C, react 6 ~ 10h.
Step 2) be in 1g:(40 ~ 60) ratio of mL, the attapulgite of acidifying is added in toluene, ultrasonic disperse 15 ~ 30min.
Step 2) in the volume ratio of the aminopropyl trimethoxysilane that adds and toluene be 3 ~ 5:100; Continuation mixing time is 12 ~ 18h.
Step 2) described in extracting be by gained solid matter absolute ethyl alcohol process 12 ~ 18h, then at 60 ~ 80 DEG C of vacuum drying 10 ~ 14h.
Step 3) in every 100mL carrene add 0.02mol ethylenediamine tetra-acetic acid; 1g step 2 is added in every 100mL carrene) obtained composite nano materials; Every 100mL carrene instillation 0.02mol thionyl chloride.
Step 3) described in washing be precipitation used carrene, acetone, distilled water, sodium bicarbonate solution (0.1M) and distilled water to wash successively.
Step 3) described in drying be carry out at 50 ~ 70 DEG C.
Chromic application in the attapulgite clay adsorbent removal industrial wastewater that method disclosed by the invention is obtained.
Chromic method in the attapulgite clay adsorbent removal water that method disclosed by the invention is obtained, adds attapulgite clay adsorbent in water to be clean, at 25 DEG C, pH value is under the condition of 3.00 ± 0.02, carries out adsorption treatment, upon adsorption reach capacity after, filter, the water be purified.
Compared with prior art, the present invention has following useful technique effect:
The preparation method of modified attapulgite earth adsorbing disclosed by the invention, first hydrochloric acid solution is adopted to carry out acidifying to attapulgite, then the attapulgite after acidifying is carried out amination process, then through ethylenediamine tetraacetic acid modified attapulgite, obtained modified attapulgite earth adsorbing.It is simple to operate, low for equipment requirements that the present invention utilizes ethylenediamine tetraacetic acid modified attapulgite to prepare the method for adsorbent; The wide material sources of attapulgite, cheap, obtained attapulgite modified adsorbent performance is good, is applicable to industrialization large-scale production.
The present invention is using ethylenediamine tetraacetic acid modified attapulgite as adsorbent, absorption method is adopted to remove trivalent chromium in water, by the carboxylic modifier of surface-functionalized introducing, utilize the complexing of ethylenediamine tetra-acetic acid and heavy metal, the trivalent chromium in Adsorption water.Adopt absorption method to remove trivalent chromium cost lower, technique is simple, and removal efficiency is high, is applicable to very much the lower trivalent chromium of concentration and removes.Therefore, the modified attapulgite earth adsorbing that the present invention obtains effectively can be applied to the trivalent chromium process of industrial wastewater.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Synthesize strong chelating agent EDTA in the present invention and modification has been carried out for attapulgite, and use it for chromic removal in water.And have no relevant report at present.
The preparation method of modified attapulgite earth adsorbing disclosed by the invention, concrete steps are as follows:
(1) acidifying of attapulgite
(2) amination of attapulgite
(3) ethylenediamine tetraacetic acid modified attapulgite
Be aminopropyl trimethoxysilane (APTES) for the silane coupler used by the attapulgite of modification in the present invention, the concrete grammar of ethylenediamine tetraacetic acid modified attapulgite clay adsorbent, as follows:
(1) acidifying of attapulgite
Take 5g attapulgite ultrasonic disperse 10 ~ 20min in the hydrochloric acid solution containing 100mL1 ~ 5mol/L, and react 6 ~ 10h at 60 ~ 80 DEG C, filter afterwards, washing, until wash neutrality, is dried, stand-by.
(2) modification of attapulgite.
The attapulgite after 2.0g acidifying is added, ultrasonic disperse 15 ~ 30min to containing in the there-necked flask of 100mL toluene (pure toluene).Under the protection of nitrogen (60mL/min), when the temperature of mixed solution is slowly risen to 110 ~ 120 DEG C, add 3 ~ 5mL aminopropyl trimethoxysilane (APTES), continue stirring 12 ~ 18h, afterwards filtration, extracting.Modified attapulgite absolute ethyl alcohol extracting 12 ~ 18h, object removes unreacted ATPES, afterwards at 60 ~ 80 DEG C of vacuum drying 12h, must test composite nano materials (APTES-ATP) used.
Under nitrogen protection; pipette the ethylenediamine tetra-acetic acid (EDTA) of 100mL carrene and 0.02mol; constant pressure dropping thionyl chloride; and add rapidly 1g ATP-APTES, react 2 ~ 3h under room temperature, filter; with carrene, acetone, distilled water, sodium acid carbonate (0.1M) solution; distilled water washs, and dry under 50 ~ 70 DEG C of conditions, obtains composite (EDTA-ATP).
The synthetic method of ethylenediamine tetraacetic acid modified attapulgite clay adsorbent is simple, and the wide material sources of attapulgite are cheap, and ethylenediamine tetraacetic acid modified attapulgite clay adsorbent has higher removal effect to trivalent chromium in water.
Utilize ethylenediamine tetraacetic acid modified attapulgite as adsorbent, adopting absorption method to remove trivalent chromium in water, is 25 DEG C in temperature, pH is under the condition of 3.00 ± 0.02, when trivalent chromium initial concentration is 80mg/L, adsorbance is 97.09mg/g, and clearance can reach 50%.Ethylenediamine tetraacetic acid modified attapulgite is used for chromic removal in water and has good economy and environment benefit by the present invention.
Embodiment 1
The preparation method of modified attapulgite earth adsorbing, concrete steps are as follows:
Take 5g attapulgite ultrasonic disperse 10min in the hydrochloric acid solution containing 100mL1mol/L, and react 6h at 80 DEG C, filter afterwards, washing, until wash neutrality, is dried, stand-by.The attapulgite after 2.0g acidifying is added, ultrasonic disperse 15min in the there-necked flask of the toluene containing 100mL.Under the protection of nitrogen (60mL/min), when the temperature of mixed solution is slowly risen to 110 DEG C, add 3mLAPTES, continue to stir 12h, afterwards filtration, extracting.Modified attapulgite absolute ethyl alcohol extracting 12h, object removes unreacted ATPES, afterwards 70 DEG C of vacuum drying 12h, must test composite nano materials (APTES-ATP) used.
Under nitrogen protection; pipette the EDTA of 100mL carrene and 0.02mol; constant pressure dropping thionyl chloride; and add rapidly 1g ATP-APTES, react 2h under room temperature, filter; with carrene, acetone, distilled water, sodium bicarbonate solution (0.1M); distilled water washs, and dry under 50 DEG C of conditions, obtains composite (EDTA-ATP).
Modified specific embodiment is as follows:
Using EDTA-ATP as adsorbent, trivalent chromium in Adsorption water.To be placed in closed container containing chromic water, add the EDTA-ATP containing trivalent chromium water quality 0.0005 times, chromic initial concentration is 50mg/L, be 25 DEG C in temperature, pH is constant temperature oscillation absorption under the condition of 3.00 ± 0.02, and adsorption time is 24h, after 24h, cross leaching filtrate, recording chromic adsorbance is 65.94mg/g, and clearance is 51.69%.
Embodiment 2
The preparation method of modified attapulgite earth adsorbing, concrete steps are as follows:
Take 5g attapulgite ultrasonic disperse 15min in the hydrochloric acid solution containing 75mL1mol/L, and react 10h at 60 DEG C, filter afterwards, washing, until wash neutrality, is dried, stand-by.The attapulgite after 2.0g acidifying is added, ultrasonic disperse 30min in the there-necked flask of the toluene containing 80mL.Under the protection of nitrogen (60mL/min), when the temperature of mixed solution is slowly risen to 120 DEG C, add 5mLAPTES, continue to stir 18h, afterwards filtration, extracting.Modified attapulgite absolute ethyl alcohol extracting 18h, object removes unreacted ATPES, afterwards 80 DEG C of vacuum drying 10h, must test composite nano materials (APTES-ATP) used.
Under nitrogen protection; pipette the EDTA of 100mL carrene and 0.02mol; constant pressure dropping thionyl chloride; and add rapidly 1g ATP-APTES, react 2h under room temperature, filter; with carrene, acetone, distilled water, sodium bicarbonate solution (0.1M); distilled water washs, and dry under 50 DEG C of conditions, obtains EDTA attapulgite modified (EDTA-ATP).
Embodiment 3
The preparation method of modified attapulgite earth adsorbing, concrete steps are as follows:
Take 5g attapulgite ultrasonic disperse 20min in the hydrochloric acid solution containing 125mL1mol/L, and react 6h at 80 DEG C, filter afterwards, washing, until wash neutrality, is dried, stand-by.The attapulgite after 2.0g acidifying is added, ultrasonic disperse 20min in the there-necked flask of the toluene containing 120mL.Under the protection of nitrogen (60mL/min), when the temperature of mixed solution is slowly risen to 120 DEG C, add 4mLAPTES, continue to stir 15h, afterwards filtration, extracting.Modified attapulgite absolute ethyl alcohol extracting 15h, object removes unreacted ATPES, afterwards 70 DEG C of vacuum drying 12h, must test composite nano materials (APTES-ATP) used.
Under nitrogen protection; pipette the EDTA of 100mL carrene and 0.02mol; constant pressure dropping thionyl chloride; and add rapidly 1g ATP-APTES, react 2h under room temperature, filter; with carrene, acetone, distilled water, sodium bicarbonate solution (0.1M); distilled water washs, and dry under 50 DEG C of conditions, obtains composite (EDTA-ATP).
Embodiment 4
With embodiment 1, take EDTA-ATP as adsorbent, when chromic initial concentration is 100mg/L, other conditions are constant, and chromic adsorbance is 111.10mg/L, and clearance is 46.44%.
Take EDTA-ATP as adsorbent, when chromic initial concentration is 140mg/L, other conditions are constant, and the chromic adsorbance of survey is 130.03mg/L, and clearance is 35.11%.
This shows, along with the increase of trivalent chromium initial concentration, adsorbent EDTA-ATP increases gradually to chromic adsorbance, and clearance reduces gradually.
Embodiment 5
With embodiment 1, take EDTA-ATP as adsorbent, when adsorption time is 35min, other conditions are constant, and adsorbent is 36.23mg/L to chromic adsorbance, and clearance is 28.98%.
Take EDTA-ATP as adsorbent, when adsorption time is 135min, other conditions are constant, and adsorbent is 48.73mg/L to chromic adsorbance, and clearance is 38.99%.
Take EDTA-ATP as adsorbent, adsorption time is 616min, and other conditions are constant, and adsorbent is 62.92mg/L to chromic adsorbance, and clearance is 50.34%.
This shows, along with increasing of adsorption time, adsorbent increases gradually to chromic adsorbance, and clearance increases gradually.
Embodiment 6
With embodiment 1, take EDTA-ATP as adsorbent, as the Ca in solution
2+concentration when being 2mmol/L, other conditions are constant, and adsorbent is 63.56mg/g to chromic adsorbance, and clearance is 48.81%.
As Ca in solution
2+concentration when being 12mmol/L, other conditions are constant, and adsorbent is 58.86mg/g to chromic adsorbance, and clearance is 47.80%
As Ca in solution
2+concentration when being 20mmol/L, other conditions are constant, and adsorbent is 51.81mg/g to chromic adsorbance, and clearance is 41.86%
This shows, Ca in solution
2+existence inhibit adsorbent to chromic absorption, along with Ca
2+the increase of solubility, adsorbent reduces gradually to chromic adsorbance, and clearance reduces gradually.
Embodiment 7
With embodiment 1, take EDTA-ATP as adsorbent, when the pH of solution is 2.43, other conditions are constant, and adsorbent is 53.93mg/g to chromic adsorbance, and clearance is 45.08%.
Take EDTA-ATP as adsorbent, when the pH of solution is 5.09, other conditions are constant, and adsorbent is 101.21mg/g to chromic adsorbance, and clearance is 78.14%.
Take EDTA-ATP as adsorbent, when the pH of solution is 5.89, other conditions are constant, and adsorbent is 126.90mg/g to chromic adsorbance, and clearance is 98.98%.
As can be seen here, along with the increase of pH value of solution, adsorbent EDTA-ATP increases gradually to chromic adsorbance, and clearance increases gradually.
Embodiment 8
With embodiment 1, be adsorbent with EDTA-ATP, when in solution, the concentration of citric acid is 20mg/L, other conditions are constant, and adsorbent is 89.78mg/g to chromic adsorbance, and clearance is 78.64%.
Be adsorbent with EDTA-ATP, when in solution, the concentration of formic acid is 20mg/L, other conditions are constant, and adsorbent is 105.71mg/g to chromic adsorbance, and clearance is 80.34%.
Be adsorbent with EDTA-ATP, when in solution, the concentration of gelatin is 20mg/L, other conditions are constant, and adsorbent is 95.19mg/g to chromic adsorbance, and clearance is 78.81%.
This shows, in solution, organic existence has good facilitation for chromic removal.
Claims (10)
1. a preparation method for modified attapulgite earth adsorbing, is characterized in that, comprises the following steps:
1) attapulgite is added in hydrochloric acid solution, ultrasonic disperse, then react at 60 ~ 80 DEG C, cross leaching precipitation, by washing of precipitate to neutral, dry, the attapulgite of obtained acidifying;
2) attapulgite of acidifying is added in toluene, ultrasonic disperse, obtain mixed solution; Then under nitrogen protection, by mixed solution by room temperature to 110 ~ 120 DEG C, add aminopropyl trimethoxysilane, continue to stir, filter, get precipitation, after will extracting being precipitated, vacuum drying, obtained composite nano materials;
3) under nitrogen protection, get carrene and ethylenediamine tetra-acetic acid, drip thionyl chloride under constant voltage, then add step 2) obtained composite nano materials, after reacting 2 ~ 3h under room temperature, cross leaching precipitation; By dry after washing of precipitate, obtained modified attapulgite earth adsorbing.
2. the preparation method of a kind of modified attapulgite earth adsorbing according to claim 1, it is characterized in that, step 1) be in 1g:(15 ~ 25) ratio of mL, attapulgite is added in the hydrochloric acid solution of 1 ~ 5mol/L, ultrasonic disperse 10 ~ 20min, then reacts 6 ~ 10h at 60 ~ 80 DEG C.
3. the preparation method of a kind of modified attapulgite earth adsorbing according to claim 1, is characterized in that, step 2) be in 1g:(40 ~ 60) ratio of mL, the attapulgite of acidifying is added in toluene, ultrasonic disperse 15 ~ 30min.
4. the preparation method of a kind of modified attapulgite earth adsorbing according to claim 1, is characterized in that, step 2) in the volume ratio of the aminopropyl trimethoxysilane that adds and toluene be 3 ~ 5:100; Continuation mixing time is 12 ~ 18h.
5. the preparation method of a kind of modified attapulgite earth adsorbing according to claim 1, is characterized in that, step 2) described in extracting be by precipitation absolute ethyl alcohol process 12 ~ 18h, then at 60 ~ 80 DEG C of vacuum drying 10 ~ 14h.
6. the preparation method of a kind of modified attapulgite earth adsorbing according to claim 1, is characterized in that, step 3) in every 100mL carrene add 0.02mol ethylenediamine tetra-acetic acid; 1g step 2 is added in every 100mL carrene) obtained composite nano materials; Every 100mL carrene instillation 0.02mol thionyl chloride.
7. the preparation method of a kind of modified attapulgite earth adsorbing according to claim 1, is characterized in that, step 3) described in washing be by precipitation successively with carrene, acetone, distilled water, sodium bicarbonate solution and distilled water washing.
8. the preparation method of a kind of modified attapulgite earth adsorbing according to claim 1, is characterized in that, step 3) described in drying be carry out at 50 ~ 70 DEG C.
9. chromic application in the attapulgite clay adsorbent removal industrial wastewater that the method in claim 1 ~ 8 described in any one is obtained.
10. the attapulgite clay adsorbent utilizing the method in claim 1 ~ 8 described in any one obtained removes chromic method in water, it is characterized in that: attapulgite clay adsorbent is added in water to be clean, at 25 DEG C, pH value is under the condition of 3.00 ± 0.02, carry out adsorption treatment, upon adsorption reach capacity after, filter, the water be purified.
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