CN110193353A - A kind of attapulgite and aniline-o-aminophenol compound adsorbent and preparation method thereof - Google Patents
A kind of attapulgite and aniline-o-aminophenol compound adsorbent and preparation method thereof Download PDFInfo
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- CN110193353A CN110193353A CN201910505754.5A CN201910505754A CN110193353A CN 110193353 A CN110193353 A CN 110193353A CN 201910505754 A CN201910505754 A CN 201910505754A CN 110193353 A CN110193353 A CN 110193353A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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Abstract
The invention belongs to adsorbent material technical fields, and in particular to a kind of attapulgite and aniline-o-aminophenol compound adsorbent and preparation method thereof: S1, pretreatment: grinding attapulgite obtains powder；S2, acidification: standing after ultrapure water stirring is added in powder, supernatant liquor be sucked out, and middle layer essence soil is taken to obtain purifying attapulgite, it purifies attapulgite and hydrochloric acid solution is added, it is centrifuged after oscillation, filter residue is filtered to obtain to suspension, washs to neutrality the attapulgite after being acidified；S3, modification: being dissolved in ethanol water for coupling agent, disperses and hydrolyzes, the attapulgite after acidification is added, and cleaning, drying obtains attapulgite modified after agitation and filtration；S4, in-situ polymerization: being dissolved in ultrapure water for aniline and hydrochloric acid, o-aminophenol and attapulgite modified slurries be added, ammonium persulfate is added after mixing, filters after reaction, washing gained filter residue to filtrate it is colourless after will be after filter residue drying grinding.Adsorbent of the invention can be effectively to the Cr(VI in waste water) it adsorbs.
Description
Technical field
The invention belongs to adsorbent material technical fields, and in particular to a kind of attapulgite and the compound suction of aniline-o-aminophenol
Attached dose and preparation method thereof.
Background technique
Chromate waste water is mainly derived from the waste water of the industries such as intermetallic composite coating, plating, process hides and paint discharge.The toxicity of chromium with
Its valence state is related, it is generally recognized that crome metal is nontoxic, Cr(III) toxicity is smaller, and Cr(VI) toxicity be Cr(III) 100 times, it is right
Organism has stronger carcinogenicity and mutagenesis characteristic.Therefore, it is necessary to control effectively and handle to chromate waste water.At present
Common chromium containing waste water treatment method includes chemical precipitation, electrolysis, reverse osmosis, ion exchange, UF membrane, absorption and bioanalysis
Deng, wherein absorption method because it is easy to operate, practical, the advantages such as advanced treating can be achieved due to be concerned, absorption method is usually adopted
Use attapulgite as adsorbent.Attapulgite is a kind of important inorganic non-metallic mine, has 3 D stereo shape skeleton structure,
There are a large amount of zeolite channels, and crystals zeolite cavity size is consistent, makes it have molecule inside crystal structure
The effect of sieve.Natural attapulgite exists in the form of stick crystalline substance beam, and stick intergranular is assembled to form aggregation.Unmodified attapulgite is inhaled
Attached dose of adsorbable polluter is many kinds of, but specific aim is not strong, and adsorption capacity is to be improved.Through peracid, modified, heat changes
Property, the modified attapulgite absorption property of surfactant-modified, silane coupler modified and macromolecular grafted etc. modes can be with
It is significantly improved, but big there are still dosage or the problems such as absorption is incomplete.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of attapulgites and aniline-o-aminophenol compound adsorbent
And preparation method thereof, can be effectively to the Cr(VI in waste water) it adsorbs.
To achieve the above object, the present invention adopts the following technical scheme:
The present invention provides a kind of attapulgites and aniline-o-aminophenol compound adsorbent preparation method, including following preparation
Step:
S1, pretreatment: then grinding attapulgite crosses 200 meshes, obtains attapulgite powder.
S2, acidification attapulgite: the attapulgite powder that step S1 is obtained is added in ultrapure water after mixing 30min
8h is stood, supernatant liquor is sucked out, middle layer essence soil is taken out and obtains purifying attapulgite, it is molten that purifying attapulgite is added to hydrochloric acid
In liquid, sonic oscillation 30min, is then added in supercentrifuge and is centrifuged, upper layer suspension is then poured out, to suspension at room temperature
Liquid filters to obtain attapulgite filter residue, the concave convex rod finally with milli-Q water attapulgite filter residue to neutrality, after being acidified
Soil, being acidified attapulgite on the one hand can be by the ratio of impurity and cation exchange increase attapulgite in removal attapulgite
On the other hand surface area can increase attapulgite absorption point, to strengthen the absorption property of attapulgite.
It is S3, attapulgite modified: coupling agent KH550 to be dissolved in the ethanol water of volume fraction 95%, stirring is allowed to equal
Even dispersion simultaneously hydrolyzes, the attapulgite after step S2 acidification is added, and 1.5h is stirred at 60 DEG C, and dehydrated alcohol is used after filtering and is surpassed
Pure water cleaning, drying obtain attapulgite modified.Hydrolysis, attapulgite easily occur for the methoxyl group in coupling agent KH550
Surface moisture rich in and hydroxyl structure, be conducive to coupling agent KH550 realization hydrolyze to form a large amount of silicone hydroxyl structure,
Silicone hydroxyl has very strong reactivity, can further be condensed with the silicone hydroxyl of attapulgite's surface, improve the suction of attapulgite
Attached performance.
S4, in-situ polymerization: aniline and hydrochloric acid are dissolved in ultrapure water, and o-aminophenol is added while stirring and step S3 is made
Attapulgite modified slurries, 30min is stirred at room temperature after mixing, the ammonium persulfate of 0.05 mol/L is then added,
8h is persistently stirred, aniline and o-aminophenol are copolymerized, are copolymerized by aniline with o-aminophenol and draw on main polymer chain
Enter specific functional groups, these functional groups are to Cr(VI) very strong suction-operated is produced, can be effectively to the Cr(VI in waste water) into
Row absorption.It is filtered after copolyreaction, and washs gained filter residue repeatedly with ultrapure water and ethyl alcohol, until by filter residue after filtrate is colourless
It is placed in 80 DEG C of vacuum ovens and dries 8h, after grinding.
The attachment behavior of attapulgite's surface silica can restrict the absorption property of attapulgite, adsorb in acidization
Know from experience in the dioxide/silica gel of attapulgite's surface and flocculation reaction occurs, the obstruction of adsorption reaction is reduced, H+To attapulgite
Acidification also continued, the absorption property of attapulgite will obtain improvement gradually, but the hydrochloric acid meeting of excessive concentrations
Cause the dissolution of attapulgite internal crystal structure, so as to cause the significant decrease of attapulgite absorption property, therefore in the present invention
In, the concentration of hydrochloric acid solution described in step S2 is 3.0mol/L.
In the present invention, the mass fraction of attapulgite modified slurries described in step S4 is 18-22%.
In the present invention, drying temperature described in step S3 is 80 DEG C -110 DEG C.
In the present invention, the concentration of aniline, hydrochloric acid and o-aminophenol described in step S4 is respectively 0.2mol/L, 0.6mol/L
And 0.3mol/L.
The present invention provides a kind of attapulgites and aniline-o-aminophenol compound adsorbent prepared by the above method.
The present invention also provides above-mentioned attapulgites and aniline-o-aminophenol compound adsorbent application method: will be described
Attapulgite and aniline-o-aminophenol compound adsorbent, which are added, contains Cr(VI) 2-4h, attapulgite and benzene is mixed in waste water
Cr(VI in amine-o-aminophenol compound adsorbent absorption waste water), reduce Cr(VI in waste water) mass concentration.
After attapulgite and aniline-o-aminophenol compound adsorbent additive amount reach certain value, attapulgite and benzene
Amine-o-aminophenol compound adsorbent is to Cr(VI) absorption basically reach balance, be further added by adsorbent additive amount adsorption effect
It will not significant change.Therefore in the present invention, the addition of waste water is added in the attapulgite and aniline-o-aminophenol compound adsorbent
Amount control is in 0.35-0.45g/L.
The size of pH value of waste water can change Cr(VI) existing forms and attapulgite and aniline-o-aminophenol composite adsorption
The charging characteristic and physicochemical property on agent surface, and then influence it to Cr(VI) removal effect.When pH value of waste water is 2-6, Cr
(VI) with HCrO in waste water4 -And Cr2O7 2-Two kinds of forms exist, while attapulgite and aniline-o-aminophenol compound adsorbent
The hydroxyl and amino on surface are by H in waste water+Proton turns to-OH2+With-NH3 +And become positively charged, thus and HCrO4 -、Cr2O7 2-Hair
The raw absorption based on electrostatic interaction, and doped anion Cl-Also easily and HCrO4 -Ion exchange occurs and removes part Cr
(VI)；When pH value of waste water is higher than 8, Cr(VI) mainly with CrO4 2-Form exists, attapulgite and aniline-in alkaline waste water
The surface protonated functional group of o-aminophenol compound adsorbent can gradually lose H+And negative electricity is taken, with CrO4 2-Generate electrostatic row
Denounce and reduce adsorbance, while CrO4 2-With Cl-It is also relatively difficult that ion exchange occurs, further results in Cr(VI) removal rate
It reduces.Therefore in the present invention, before attapulgite and aniline-o-aminophenol compound adsorbent being added, the pH value of waste water is adjusted to
4-6。
The invention has the following beneficial effects:
The present invention is first acidified attapulgite powder, and acidification attapulgite on the one hand can be by removal attapulgite
Impurity and cation exchange increase the specific surface area of attapulgite, on the other hand can increase attapulgite absorption point, thus
Strengthen the absorption property of attapulgite.Attapulgite powder is modified using Silane coupling agent KH550 after acidification, coupling agent
Hydrolysis, the surface of attapulgite moisture rich in and hydroxyl structure easily occur for the methoxyl group in KH550, are conducive to
Coupling agent KH550 realization hydrolyzes to form a large amount of silicone hydroxyl structure, and silicone hydroxyl has very strong reactivity, can be with attapulgite
The silicone hydroxyl on surface is further condensed, and further increases the absorption property of attapulgite.It will be modified recessed finally by in-situ polymerization
Convex stick soil, aniline and o-aminophenol are copolymerized and attapulgite and aniline-o-aminophenol compound adsorbent are made, and pass through aniline and adjacent ammonia
Base phenol, which is copolymerized on main polymer chain, introduces specific functional groups, these functional groups are to Cr(VI) very strong suction-operated is produced,
Can be effectively to the Cr(VI in waste water) it adsorbs.
Specific embodiment
Present invention will be further explained below with reference to specific examples.These embodiments are merely to illustrate the present invention and do not have to
In limiting the scope of the invention.
Embodiment 1
Present embodiments provide a kind of attapulgite and aniline-o-aminophenol compound adsorbent 1 preparation method, including following system
Standby step:
S1, pretreatment: then grinding attapulgite crosses 200 meshes, obtains attapulgite powder；
S2, acidification attapulgite: the attapulgite powder that step S1 is obtained is added in ultrapure water after 30min is mixed and is stood
Supernatant liquor is sucked out in 8h, takes out middle layer essence soil and obtains purifying attapulgite, and purifying attapulgite is added to concentration
In the hydrochloric acid solution of 3.0mol/L, sonic oscillation 30min, is then added in supercentrifuge and is centrifuged, then pour out at room temperature
Upper layer suspension filters suspension to obtain attapulgite filter residue, is finally obtained with milli-Q water attapulgite filter residue to neutrality
Attapulgite after to acidification；
It is S3, attapulgite modified: coupling agent KH550 to be dissolved in the ethanol water of volume fraction 95%, stirring is allowed to uniformly point
It dissipates and hydrolyzes, the attapulgite after step S2 acidification is added stirs 1.5h at 60 DEG C, dehydrated alcohol and ultrapure water are used after filtering
Cleaning, drying obtains attapulgite modified under the conditions of 80 DEG C of temperature；
S4, in-situ polymerization: by concentration be 0.2mol/L aniline and concentration be 0.6mol/L hydrochloric acid be dissolved in ultrapure water, while stirring
It mixes side and attapulgite modified slurries made from the o-aminophenol and step S3 that concentration is 0.3mol/L, modified attapulgite soil paste is added
The mass fraction of liquid is 18%, and 30min is stirred at room temperature after mixing, the ammonium persulfate of 0.05 mol/L is then added, holds
Continuous stirring 8h, filters after reaction, and washs gained filter residue repeatedly with ultrapure water and ethyl alcohol, until setting filter residue after filtrate is colourless
8h is dried in 80 DEG C of vacuum ovens, attapulgite and aniline-o-aminophenol compound adsorbent 1 are made after grinding.
Present embodiments provide attapulgite and aniline-o-aminophenol compound adsorbent 1 application method: by the pH of waste water
Value is adjusted to 4, and attapulgite and aniline-o-aminophenol compound adsorbent 1 is added by the dosage of 0.35g/L and contains Cr(VI) it is useless
2h is mixed in water, attapulgite and aniline-o-aminophenol compound adsorbent 1 adsorb the Cr(VI in waste water), reduce waste water
Middle Cr(VI) mass concentration.
Embodiment 2
Present embodiments provide a kind of attapulgite and aniline-o-aminophenol compound adsorbent 2 preparation method, including following system
Standby step:
S1, pretreatment: then grinding attapulgite crosses 200 meshes, obtains attapulgite powder；
S2, acidification attapulgite: the attapulgite powder that step S1 is obtained is added in ultrapure water after 30min is mixed and is stood
Supernatant liquor is sucked out in 8h, takes out middle layer essence soil and obtains purifying attapulgite, and purifying attapulgite is added to concentration
In the hydrochloric acid solution of 3.0mol/L, sonic oscillation 30min, is then added in supercentrifuge and is centrifuged, then pour out at room temperature
Upper layer suspension filters suspension to obtain attapulgite filter residue, is finally obtained with milli-Q water attapulgite filter residue to neutrality
Attapulgite after to acidification；
It is S3, attapulgite modified: coupling agent KH550 to be dissolved in the ethanol water of volume fraction 95%, stirring is allowed to uniformly point
It dissipates and hydrolyzes, the attapulgite after step S2 acidification is added stirs 1.5h at 60 DEG C, dehydrated alcohol and ultrapure water are used after filtering
Cleaning, drying obtains attapulgite modified under the conditions of 95 DEG C of temperature；
S4, in-situ polymerization: by concentration be 0.2mol/L aniline and concentration be 0.6mol/L hydrochloric acid be dissolved in ultrapure water, while stirring
It mixes side and attapulgite modified slurries made from the o-aminophenol and step S3 that concentration is 0.3mol/L, modified attapulgite soil paste is added
The mass fraction of liquid is 20%, and 30min is stirred at room temperature after mixing, the ammonium persulfate of 0.05 mol/L is then added, holds
Continuous stirring 8h, filters after reaction, and washs gained filter residue repeatedly with ultrapure water and ethyl alcohol, until setting filter residue after filtrate is colourless
8h is dried in 80 DEG C of vacuum ovens, attapulgite and aniline-o-aminophenol compound adsorbent 2 are made after grinding.
Present embodiments provide attapulgite and aniline-o-aminophenol compound adsorbent 2 application method: by the pH of waste water
Value is adjusted to 5, and attapulgite and aniline-o-aminophenol compound adsorbent 2 is added by the additive amount of 0.4g/L and contains Cr(VI) it is useless
3h is mixed in water, attapulgite and aniline-o-aminophenol compound adsorbent 2 adsorb the Cr(VI in waste water), reduce waste water
Middle Cr(VI) mass concentration.
Embodiment 3
Present embodiments provide a kind of attapulgite and aniline-o-aminophenol compound adsorbent 3 preparation method, including following system
Standby step:
S1, pretreatment: then grinding attapulgite crosses 200 meshes, obtains attapulgite powder；
S2, acidification attapulgite: the attapulgite powder that step S1 is obtained is added in ultrapure water after 30min is mixed and is stood
Supernatant liquor is sucked out in 8h, takes out middle layer essence soil and obtains purifying attapulgite, and purifying attapulgite is added to concentration
In the hydrochloric acid solution of 3.0mol/L, sonic oscillation 30min, is then added in supercentrifuge and is centrifuged, then pour out at room temperature
Upper layer suspension filters suspension to obtain attapulgite filter residue, is finally obtained with milli-Q water attapulgite filter residue to neutrality
Attapulgite after to acidification；
It is S3, attapulgite modified: coupling agent KH550 to be dissolved in the ethanol water of volume fraction 95%, stirring is allowed to uniformly point
It dissipates and hydrolyzes, the attapulgite after step S2 acidification is added stirs 1.5h at 60 DEG C, dehydrated alcohol and ultrapure water are used after filtering
Cleaning, drying obtains attapulgite modified under the conditions of 110 DEG C of temperature；
S4, in-situ polymerization: by concentration be 0.2mol/L aniline and concentration be 0.6mol/L hydrochloric acid be dissolved in ultrapure water, while stirring
It mixes side and attapulgite modified slurries made from the o-aminophenol and step S3 that concentration is 0.3mol/L, modified attapulgite soil paste is added
The mass fraction of liquid is 22%, and 30min is stirred at room temperature after mixing, the ammonium persulfate of 0.05 mol/L is then added, holds
Continuous stirring 8h, filters after reaction, and washs gained filter residue repeatedly with ultrapure water and ethyl alcohol, until setting filter residue after filtrate is colourless
8h is dried in 80 DEG C of vacuum ovens, attapulgite and aniline-o-aminophenol compound adsorbent 3 are made after grinding.
Present embodiments provide attapulgite and aniline-o-aminophenol compound adsorbent 3 application method: by the pH of waste water
Value is adjusted to 6, and attapulgite and aniline-o-aminophenol compound adsorbent 3 is added by the additive amount of 0.45g/L and contains Cr(VI) it is useless
2-4h is mixed in water, attapulgite and aniline-o-aminophenol compound adsorbent 3 adsorb the Cr(VI in waste water), it reduces useless
Cr(VI in water) mass concentration.
Comparative example 1
This comparative example provides a kind of preparation method of modified attapulgite earth adsorbing 4, including following preparation step:
S1, pretreatment: then grinding attapulgite crosses 200 meshes, obtains attapulgite powder；
S2, acidification attapulgite: the attapulgite powder that step S1 is obtained is added in ultrapure water after 30min is mixed and is stood
Supernatant liquor is sucked out in 8h, takes out middle layer essence soil and obtains purifying attapulgite, and purifying attapulgite is added to concentration
In the hydrochloric acid solution of 3.0mol/L, sonic oscillation 30min, is then added in supercentrifuge and is centrifuged, then pour out at room temperature
Upper layer suspension filters suspension to obtain attapulgite filter residue, is finally obtained with milli-Q water attapulgite filter residue to neutrality
Attapulgite after to acidification；
S3, modified attapulgite earth adsorbing: coupling agent KH550 is dissolved in the ethanol water of volume fraction 95%, stirring is allowed to
Evenly dispersed and hydrolyze, after step S2 acidification is added attapulgite, stirs 1.5h at 60 DEG C, after filtering with dehydrated alcohol and
Ultrapure water cleaning, drying obtains modified attapulgite earth adsorbing 4 under the conditions of 110 DEG C of temperature.
This comparative example provides the application method of modified attapulgite earth adsorbing 4: modified attapulgite earth adsorbing 4 is added
Containing Cr(VI) 4h is mixed in waste water, modified attapulgite earth adsorbing 4 adsorbs the Cr(VI in waste water), reduce Cr in waste water
(VI) mass concentration.
Comparative example 2
This comparative example provides a kind of attapulgite and aniline-o-aminophenol compound adsorbent 5 preparation method, including following system
Standby step:
S1, pretreatment: then grinding attapulgite crosses 200 meshes, obtains attapulgite powder；
S2, acidification attapulgite: the attapulgite powder that step S1 is obtained is added in ultrapure water after 30min is mixed and is stood
Supernatant liquor is sucked out in 8h, takes out middle layer essence soil and obtains purifying attapulgite, and purifying attapulgite is added to concentration
In the hydrochloric acid solution of 3.0mol/L, sonic oscillation 30min, is then added in supercentrifuge and is centrifuged, then pour out at room temperature
Upper layer suspension filters suspension to obtain attapulgite filter residue, is finally obtained with milli-Q water attapulgite filter residue to neutrality
Attapulgite after to acidification；
It is S3, attapulgite modified: coupling agent KH550 to be dissolved in the ethanol water of volume fraction 95%, stirring is allowed to uniformly point
It dissipates and hydrolyzes, the attapulgite after step S2 acidification is added stirs 1.5h at 60 DEG C, dehydrated alcohol and ultrapure water are used after filtering
Cleaning, drying obtains attapulgite modified under the conditions of 110 DEG C of temperature；
S4, in-situ polymerization: by concentration be 0.2mol/L aniline and concentration be 0.6mol/L hydrochloric acid be dissolved in ultrapure water, while stirring
It mixes side and attapulgite modified slurries made from the o-aminophenol and step S3 that concentration is 0.3mol/L, modified attapulgite soil paste is added
The mass fraction of liquid is 22%, and 30min is stirred at room temperature after mixing, the ammonium persulfate of 0.05 mol/L is then added, holds
Continuous stirring 8h, filters after reaction, and washs gained filter residue repeatedly with ultrapure water and ethyl alcohol, until setting filter residue after filtrate is colourless
8h is dried in 80 DEG C of vacuum ovens, attapulgite and aniline-o-aminophenol compound adsorbent 5 are made after grinding.
This comparative example provides attapulgite and aniline-o-aminophenol compound adsorbent 5 application method: by 0.2g/L's
Attapulgite and aniline-o-aminophenol compound adsorbent 5 are added additive amount contains Cr(VI) 4h, concave convex rod is mixed in waste water
Soil and aniline-o-aminophenol compound adsorbent 5 adsorb the Cr(VI in waste water), reduce Cr(VI in waste water) mass concentration.
Taking 5 groups of 1L initial mass concentration respectively is the Cr(VI of 50 mg/L) solution, solution is numbered.By embodiment
Adsorbent prepared by 1-3, comparative example 1 and comparative example 2 is added in 1-5 solution according to the application method, in 25 DEG C of temperature
Under the conditions of 2h is mixed, then with 0.45 μm of membrane filtration and measure Cr(VI in filtrate) mass concentration, calculate Cr(VI) go
Except rate, as a result as shown in table 1 below:
Table 1
| Test item | No. 1 solution | No. 2 solution | No. 3 solution | No. 4 solution | No. 5 solution |
| Cr(VI) final mass concentration (mg/L) | 4.23 | 3.98 | 3.37 | 22.89 | 18.63 |
| Cr(VI) removal rate (%) | 91.55 | 92.04 | 93.27 | 54.23 | 62.74 |
No. 1 solution, No. 2 solution and No. 3 solution C r(VI) final mass concentration will be significantly lower than No. 4 solution；No. 5 solution C r(VI)
Final mass concentration is slightly below No. 4 solution, but is apparently higher than No. 1 solution, No. 2 solution and No. 3 solution C r(VI) final mass is dense
Degree, illustrates attapulgite prepared by embodiment 1-3 and aniline-o-aminophenol compound adsorbent, changes compared to prepared by comparative example 1
Property adsorbent is to Cr(VI) adsorption capacity it is stronger, according to application method described in embodiment 1-3 to Cr(VI in solution) inhale
It is attached, there is better adsorption effect compared to by application method described in comparative example 2.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (9)
1. a kind of attapulgite and aniline-o-aminophenol compound adsorbent preparation method, it is characterised in that: including following preparation
Step:
S1, pretreatment: then grinding attapulgite crosses 200 meshes, obtains attapulgite powder；
S2, acidification attapulgite: the attapulgite powder that step S1 is obtained is added in ultrapure water after 30min is mixed and is stood
Supernatant liquor is sucked out in 8h, takes out middle layer essence soil and obtains purifying attapulgite, and purifying attapulgite is added to hydrochloric acid solution
In, sonic oscillation 30min, is then added in supercentrifuge and is centrifuged, upper layer suspension is then poured out, to suspension at room temperature
Suction filtration obtains attapulgite filter residue, the attapulgite finally with milli-Q water attapulgite filter residue to neutrality, after being acidified；
It is S3, attapulgite modified: coupling agent KH550 to be dissolved in the ethanol water of volume fraction 95%, stirring is allowed to uniformly point
It dissipates and hydrolyzes, the attapulgite after step S2 acidification is added stirs 1.5h at 60 DEG C, dehydrated alcohol and ultrapure water are used after filtering
Cleaning, drying obtain attapulgite modified；
S4, in-situ polymerization: aniline and hydrochloric acid are dissolved in ultrapure water, are added made from o-aminophenol and step S3 and are changed while stirring
Property attapulgite slurry, 30min is stirred at room temperature after mixing, the ammonium persulfate of 0.05 mol/L is then added, continue
8h is stirred, is filtered after reaction, and washs gained filter residue repeatedly with ultrapure water and ethyl alcohol, until being placed in filter residue after filtrate is colourless
8h is dried in 80 DEG C of vacuum ovens, after grinding.
2. a kind of attapulgite and aniline-o-aminophenol compound adsorbent preparation method according to claim 1, feature
Be: the concentration of hydrochloric acid solution described in step S2 is 3.0mol/L.
3. a kind of attapulgite and aniline-o-aminophenol compound adsorbent preparation method according to claim 1, feature
Be: the mass fraction of attapulgite modified slurries described in step S4 is 18-22%.
4. a kind of attapulgite and aniline-o-aminophenol compound adsorbent preparation method according to claim 1, feature
Be: drying temperature described in step S3 is 80 DEG C -110 DEG C.
5. a kind of attapulgite and aniline-o-aminophenol compound adsorbent preparation method according to claim 1, feature
Be: the concentration of aniline described in step S4, hydrochloric acid and o-aminophenol is respectively 0.2mol/L, 0.6mol/L and 0.3mol/L.
6. a kind of attapulgite and aniline-o-aminophenol compound adsorbent, it is characterised in that: the attapulgite and aniline-neighbour
Amino phenols compound adsorbent preparation method as described in claim 1 is prepared.
7. a kind of attapulgite and aniline-o-aminophenol compound adsorbent application method according to claim 6, feature
It is: the attapulgite and aniline-o-aminophenol compound adsorbent is added containing 2-4h is mixed in Cr(VI) waste water, it is recessed
Cr(VI in convex stick soil and aniline-o-aminophenol compound adsorbent absorption waste water), reduce Cr(VI in waste water) mass concentration.
8. a kind of attapulgite and aniline-o-aminophenol compound adsorbent application method according to claim 7, feature
Be: the additive amount control of waste water is added in 0.35-0.45g/L in the attapulgite and aniline-o-aminophenol compound adsorbent.
9. a kind of attapulgite and aniline-o-aminophenol compound adsorbent application method according to claim 7, feature
It is: before attapulgite and aniline-o-aminophenol compound adsorbent is added, the pH value of waste water is adjusted to 4-6.
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| CN115350685A (en) * | 2022-08-16 | 2022-11-18 | 青海师范大学 | Attapulgite composite material rich in ortho-position hydroxyl as well as preparation method and application thereof |
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| CN115350685A (en) * | 2022-08-16 | 2022-11-18 | 青海师范大学 | Attapulgite composite material rich in ortho-position hydroxyl as well as preparation method and application thereof |
| CN115350685B (en) * | 2022-08-16 | 2024-01-23 | 青海师范大学 | Attapulgite composite material rich in ortho-hydroxyl and preparation method and application thereof |
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Application publication date: 20190903 |