CN106943984A - A kind of arsenic-removing adsorption agent and preparation method thereof - Google Patents
A kind of arsenic-removing adsorption agent and preparation method thereof Download PDFInfo
- Publication number
- CN106943984A CN106943984A CN201710228854.9A CN201710228854A CN106943984A CN 106943984 A CN106943984 A CN 106943984A CN 201710228854 A CN201710228854 A CN 201710228854A CN 106943984 A CN106943984 A CN 106943984A
- Authority
- CN
- China
- Prior art keywords
- arsenic
- magnesium
- preparation
- adsorption agent
- removing adsorption
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to a kind of preparation method of arsenic-removing adsorption agent, belong to environmentally conscious materials field, the preparation method comprises the following steps successively：The preparation of magnalium hydrotalcite；The introducing of intercalation hydrogen peroxide between laminate；Heterogeneous class Fenton's reaction；Pickling.The material can be applied to the Adsorption of arsenic in water as adsorbent.Preparation technology of the present invention is simple, with low cost, the features such as obtained material has orderly mesopore orbit, uniform particle diameter, higher specific surface area and pore volume, adsorbent made from the inventive method can large-scale application in waste water arsenic efficient removal and be easy to regeneration.
Description
Technical field
The invention belongs to environmentally conscious materialses technical field, more particularly to a kind of arsenic-removing adsorption agent and its preparation method and application.
Background technology
Heavy metal pollution problem, especially arsenic pollution are always the environmental problem of people's common concern.Arsenic pollution is not only tight
Heavy compromises environment, and the also production, life and human health or safety to local resident causes serious harm.2011
Year, first " the 12 " ad hoc planning of China-《Heavy metal pollution integrated control " 12 " is planned》Arsenic planning power has been included in
Seek one of heavy metal of control.
At present, mainly there are absorption method, bioanalysis, ion-exchange, membrane separation process to the administering method of arsenic pollution both at home and abroad
Deng.Compared with other method absorption method have efficiently, easy and good selective, it is particularly strong to low concentration, contaminative,
The processing of the big arsenic-containing waste water of toxicity is with unique application value.The conventional adsorbent of absorption method processing arsenic-containing waste water mainly may be used
To be divided into：（1）Biomaterial：Mushroom, algae, activated sludge and agricultural by product and agricultural wastes etc.；（2）Inorganic matter and ore deposit
Material：Flyash, zeolite, activated carbon, bentonite, sepiolite etc.；（3）Organic compound：Chitosan, polyaniline etc.；（4）Have
Machine-inorganic composite：Bentonite-chitosan, natural zeolite loading chitosan, poly- diethyl annulated pyridine modified alta-mud etc..But
Processing of the existing adsorbent to arsenic-containing waste water has that capacity is small and the rate of adsorption is slowly etc. not enough, mainly due to these adsorbent ratios
Surface area is small, pore volume is small, dynamics is disperseed caused by the reason such as uneven.
The content of the invention
The purpose of the present invention is a kind of even particle size distribution of exploitation, with high-specific surface area and pore volume and be easy to regeneration
Arsenic-removing adsorption agent, while a kind of preparation method simple to operate of above-mentioned arsenic-removing adsorption agent is provided, to overcome existing arsenic removal to adsorb
The problem of agent adsorption capacity is small, the rate of adsorption slow and is difficult to regenerate.
To reach above-mentioned purpose, the technical proposal of the invention is realized in this way：
A kind of preparation method of arsenic-removing adsorption agent, comprises the following steps：
Step one：Prepare magnalium hydrotalcite powder；
Step 2：Concentration is placed in beaker for 30%-50% hydrogen peroxide, and is rapidly added stabilizer, is placed in ice bath and stirs
Obtain dioxygen water mixed liquid.
Step 3：The magnalium hydrotalcite powder obtained by step one is added into the dioxygen water mixed liquid described in step 2, it is whole
Individual adition process is maintained under ice bath environment and is stirred continuously；
Step 4：Step 3 products therefrom is subjected to suction filtration, then with ethyl alcohol recrystallization twice, dried at room temperature, sealing is protected
Deposit；
Step 5：Water intaking, adds after ferrous salt or molysite, stirring and dissolving into water, step 4 products therefrom is added into water, whole
Individual process is kept stirring for, and the reaction time is 20 ~ 100 minutes；
Step 6：Step 5 products therefrom is subjected to suction filtration, after weak acid scrubbing 2 times, neutrality is washed with deionized, in
Room temperature ~ 100 DEG C are dried, sealing preserve.
Magnalium hydrotalcite powder is prepared in the step one and specifically includes following steps：
Step（1）：Prepare the magnesium-aluminum metal mixed salt solution that molar concentration is 1 ~ 1.2 mol/L, the magnesium-aluminum metal salt mixing
The molar ratio range of magnesium and aluminium is 2 in solution:3~5:1；
Step（2）：Prepare the molar concentration of sodium carbonate in the mixed ammonium/alkali solutions that NaOH and sodium carbonate are constituted, mixed ammonium/alkali solutions
For 2 times of aluminium salt concentration in magnesium-aluminum metal mixed salt solution, the molar concentration of NaOH is in magnesium-aluminum metal mixed salt solution
1.6 times of metal ion total concentration；
Step（3）：Magnesium-aluminum metal mixed salt solution is instilled in deionized water with mixed ammonium/alkali solutions with identical constant drop speed, it is whole
Individual titration process is kept stirring for；
Step（4）：Continue to stir uniform to solution after the completion of titration, 3 ~ 24h is stood until solution crystallization at 60 ~ 180 DEG C；
Step（5）：The mixed liquor that crystallization is completed carries out suction filtration, and solid obtained by suction filtration is washed with deionized totally, then made
Use ethyl alcohol recrystallization；
Step（6）：The solid of recrystallization is dried, drying product is ground, magnalium hydrotalcite powder is obtained.
The step（1）In magnesium-aluminum metal mixed salt solution be magnesium sulfate aluminium salt, magnesium nitrate aluminium salt, chlorine magnalium salt, carbon
One or more of combinations of sour magnalium salt.
The stabilizer added in the step 2 selects magnesium sulfate, magnesium nitrate, sodium stannate, one kind of organic phosphate, surely
The proportion for determining agent and hydrogen peroxide is 0.3:100~0.6:100；
The mass ratio of hydrogen peroxide and magnalium hydrotalcite powder is more than 7 in the step 3.
In the step 5 ferrous salt from ferrous sulfate or frerrous chloride one kind, molysite from ferric sulfate, iron chloride,
One kind of ferric nitrate.
Dilute acid concentration used in the step 6 is less than 0.2 mol/L, and diluted acid is the one of sulfuric acid, hydrochloric acid or nitric acid
Kind.
The arsenic-removing adsorption agent according to made from above-mentioned preparation method.
The arsenic-removing adsorption agent according to made from above-mentioned preparation method pollutes the application of Adsorption in arsenic in water body.
Compared with prior art, beneficial effects of the present invention：
1st, the present invention obtained by arsenic-removing adsorption agent there is larger specific surface area, pore volume, its even particle size distribution, particle diameter compared with
It is small, with preferable stability, memory effect and environment-friendly characteristic；
2nd, the raw material of product of the present invention is easy to get, and preparation technology is simple, and whole preparation process is carried out under atmospheric atmosphere, without lazy
Property gas shield, prepare it is with low cost, the need for industrialized production and use can be met；
3rd, the use scope of product of the present invention is more extensive, is applicable to pH 2 ~ 12 broad range, and adsorption reaction speed is fast,
The quick adsorption that arsenic in water body can be achieved is removed.
4th, product of the present invention can regenerate, it is only necessary to which simple step can regenerate, and the product after regeneration for several times is still
So there is good using effect.
Figure of description
Fig. 1 is the microscopic appearance figure of magnalium hydrotalcite prepared by low saturation coprecipitation；
Fig. 2 is the microscopic appearance figure of arsenic-removing adsorption agent produced by the present invention.
Embodiment
The present invention is described in further detail with specific implementation example below in conjunction with the accompanying drawings, but the protection model of the present invention
Enclose be not limited to it is as described below：
The method comprises the steps of firstly, preparing magnalium hydrotalcite, hydrogen peroxide is then introduced by magnalium hydrotalcite layer using improvement the crystallizing process under low temperature
Between plate, it is combined with carbonate in the form of hydrogen bond, then it is handled under Fenton environment, products therefrom can be used for giving up
The efficient absorption of arsenic is removed in water.
The scanning electron microscope (SEM) photograph difference of magnalium hydrotalcite and product arsenic-removing adsorption agent of the present invention is as illustrated in fig. 1 and 2；Can by Fig. 1
Know, the magnalium hydrotalcite prepared using traditional low saturation coprecipitation has lamellar structure, but particle diameter distribution is uneven.By scheming
2 understand, the arsenic-removing adsorption agent for preparing of the present invention also has lamellar structure, and lamella edge clear, crystallinity is higher, and particle compared with
Small, particle diameter distribution is uniform.
Several embodiments of the present invention are described below：
Embodiment 1
A kind of preparation method of arsenic-removing adsorption agent, the described method comprises the following steps：
Step one：Prepare in the magnesium-aluminum metal mixed salt solution that molar concentration is 1mol/L, the magnesium-aluminum metal mixed salt solution
The molar ratio range of magnesium and aluminium is 2:3；Magnesium-aluminum metal salt is magnesium nitrate and aluminum nitrate.
Step 2：Prepare mole of sodium carbonate in the mixed ammonium/alkali solutions that NaOH and sodium carbonate are constituted, mixed ammonium/alkali solutions
Concentration is 2 times of aluminium salt concentration in magnesium-aluminum metal mixed salt solution, and the molar concentration of NaOH mixes molten for magnesium-aluminum metal salt
1.6 times of metal ion total concentration in liquid；
Step 3：Magnesium-aluminum metal mixed salt solution is instilled in deionized water with mixed ammonium/alkali solutions with identical constant drop speed, it is whole
Individual titration process is kept stirring for；
Step 4：Continue to stir uniform to solution after the completion of titration, 24h is stood until solution crystallization at 60 DEG C；
Step 5：The mixed liquor that crystallization is completed carries out suction filtration, and solid obtained by suction filtration is washed with deionized totally, then used
Ethyl alcohol recrystallization；
Step 6：The solid of recrystallization is dried, drying product is ground, magnalium hydrotalcite powder is obtained；
Step 7：Concentration is placed in beaker for 30% hydrogen peroxide, and is rapidly added stabilizer, stirring in ice bath is placed in and obtains
Dioxygen water mixed liquid, prevents decomposing hydrogen dioxide solution, and stabilizer selects magnesium sulfate, and the ratio of stabilizer and hydrogen peroxide is 0.3:100；
Step 8：The magnalium hydrotalcite powder obtained by step 6 is added into the dioxygen water mixed liquid described in step 7, it is whole to add
Enter process to be maintained under ice bath environment and be stirred continuously；The mass ratio of hydrogen peroxide and magnalium hydrotalcite powder is more than 7.
Step 9：Step 8 products therefrom is subjected to suction filtration, then with ethyl alcohol recrystallization twice, dried at room temperature, it is close
Envelope is preserved；
Step 10：Water intaking regulation pH is 2, is added into water after ferrous sulfate, stirring and dissolving, and production obtained by step 9 is added into water
Thing, whole process is kept stirring for, and the reaction time is 20 minutes；
Step 11：Step 10 products therefrom is subjected to suction filtration, after being washed 2 times using dilute sulfuric acid, in being washed with deionized
Property, in room temperature drying, sealing preserve；Dilute sulfuric acid concentration is less than 0.2 mol/L.
Embodiment 2
A kind of preparation method of arsenic-removing adsorption agent, the described method comprises the following steps：
Step one：Prepare the magnesium-aluminum metal mixed salt solution that molar concentration is 1.2mol/L, the magnesium-aluminum metal mixed salt solution
The molar ratio range of middle magnesium and aluminium is 5:1；Magnesium-aluminum metal salt is aluminum nitrate and magnesium nitrate.
Step 2：Prepare mole of sodium carbonate in the mixed ammonium/alkali solutions that NaOH and sodium carbonate are constituted, mixed ammonium/alkali solutions
Concentration is 2 times of aluminium salt concentration in magnesium-aluminum metal mixed salt solution, and the molar concentration of NaOH mixes molten for magnesium-aluminum metal salt
1.6 times of metal ion total concentration in liquid；
Step 3：Magnesium-aluminum metal mixed salt solution is instilled in deionized water with mixed ammonium/alkali solutions with identical constant drop speed, it is whole
Individual titration process is kept stirring for；
Step 4：Continue to stir uniform to solution after the completion of titration, 3h is stood until solution crystallization at 180 DEG C；
Step 5：The mixed liquor that crystallization is completed carries out suction filtration, and solid obtained by suction filtration is washed with deionized totally, then used
Ethyl alcohol recrystallization；
Step 6：The solid of recrystallization is dried, drying product is ground, magnalium hydrotalcite powder is obtained；
Step 7：Concentration is placed in beaker for 50% hydrogen peroxide, and is rapidly added stabilizer, stirring in ice bath is placed in and obtains
Dioxygen water mixed liquid, prevents decomposing hydrogen dioxide solution, and stabilizer selects sodium stannate, and the ratio of stabilizer and hydrogen peroxide is 0.6:100；
Step 8：The magnalium hydrotalcite powder obtained by step 6 is added into the dioxygen water mixed liquid described in step 7, it is whole to add
Enter process to be maintained under ice bath environment and be stirred continuously；The mass ratio of hydrogen peroxide and magnalium hydrotalcite powder is more than 7.
Step 9：Step 8 products therefrom is subjected to suction filtration, then with ethyl alcohol recrystallization twice, dried at room temperature, it is close
Envelope is preserved；
Step 10：Water intaking regulation pH is 13, is added into water after ferric sulfate, stirring and dissolving, and production obtained by step 9 is added into water
Thing, whole process is kept stirring for, and the reaction time is 100 minutes；
Step 11：Step 10 products therefrom is subjected to suction filtration, after being washed 2 times using dilute sulfuric acid, in being washed with deionized
Property, in 100 DEG C of drying, sealing preserve；Dilute sulfuric acid concentration is less than 0.2 mol/L.
Embodiment 3
A kind of preparation method of arsenic-removing adsorption agent, the described method comprises the following steps：
Step one：Prepare the magnesium-aluminum metal mixed salt solution that molar concentration is 1.1 mol/L, the magnesium-aluminum metal mixed salt solution
The molar ratio range of middle magnesium and aluminium is 2:1；Magnesium-aluminum metal salt is aluminum sulfate and magnesium chloride.
Step 2：Prepare mole of sodium carbonate in the mixed ammonium/alkali solutions that NaOH and sodium carbonate are constituted, mixed ammonium/alkali solutions
Concentration is 2 times of aluminium salt concentration in magnesium-aluminum metal mixed salt solution, and the molar concentration of NaOH mixes molten for magnesium-aluminum metal salt
1.6 times of metal ion total concentration in liquid；
Step 3：Magnesium-aluminum metal mixed salt solution is instilled in deionized water with mixed ammonium/alkali solutions with identical constant drop speed, it is whole
Individual titration process is kept stirring for；
Step 4：Continue to stir uniform to solution after the completion of titration, 15h is stood until solution crystallization at 120 DEG C；
Step 5：The mixed liquor that crystallization is completed carries out suction filtration, and solid obtained by suction filtration is washed with deionized totally, then used
Ethyl alcohol recrystallization；
Step 6：The solid of recrystallization is dried, drying product is ground, magnalium hydrotalcite powder is obtained；
Step 7：Concentration is placed in beaker for 40% hydrogen peroxide, and is rapidly added stabilizer, stirring in ice bath is placed in and obtains
Dioxygen water mixed liquid, prevents decomposing hydrogen dioxide solution, and stabilizer selects magnesium nitrate, and the ratio of stabilizer and hydrogen peroxide is 0.5:100；
Step 8：The magnalium hydrotalcite powder obtained by step 6 is added into the dioxygen water mixed liquid described in step 7, it is whole to add
Enter process to be maintained under ice bath environment and be stirred continuously；The mass ratio of hydrogen peroxide and magnalium hydrotalcite powder is more than 7.
Step 9：Step 8 products therefrom is subjected to suction filtration, then with ethyl alcohol recrystallization twice, dried at room temperature, it is close
Envelope is preserved；
Step 10：Water intaking regulation pH is 7, and ferrous sulfate is added into water；After stirring and dissolving, production obtained by step 9 is added into water
Thing, whole process is kept stirring for, and the reaction time is 60 minutes；
Step 11：Step 10 products therefrom is subjected to suction filtration, after being washed 2 times using dilute sulfuric acid, in being washed with deionized
Property, in 60 DEG C of drying, sealing preserve；Dilute sulfuric acid concentration is less than 0.2 mol/L.
Arsenic-removing adsorption agent prepared by embodiment 1-3 is applied to the Adsorption of pentavalent arsenic.200 mL are added in the reactor
10mg/L As5+Solution, adjusts pH value of solution, and 0.05 g arsenic-removing adsorption agents are added into solution, opens stirring, reacts 10 minutes,
It the results are shown in Table 1.
The Adsorption experiment of the pentavalent arsenic of table 1
The arsenic-removing adsorption agent of the present invention is easy to regeneration, reusable.
Solution after the completion of embodiment 3 is reacted is filtered, and gained solid matter is washed using dilute sulfuric acid, is dried
It is dry, regeneration（The step 10 of above-described embodiment ~ 11）.Arsenic-removing adsorption agent after regeneration is re-used for 10mg/L As5+Solution
Processing, adjusts 200 mLAs5+PH value of solution is 6.01, and 0.05 g arsenic-removing adsorption agents are added into solution, opens stirring, reaction 10
After minute, As in solution5+Clearance be 99.63%.The arsenic-removing adsorption agent is reclaimed, regenerated, after reusing 3 times, in solution
As5+Clearance still up to 98.46%.
Present disclosure is not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention
And any equivalent conversion taken technical solution of the present invention, it is claim of the invention and is covered.
Claims (9)
1. a kind of preparation method of arsenic-removing adsorption agent, it is characterised in that：It the described method comprises the following steps：
Step one：Prepare magnalium hydrotalcite powder；
Step 2：Concentration is placed in beaker for 30%-50% hydrogen peroxide, and is rapidly added stabilizer, is placed in ice bath and stirs
Obtain dioxygen water mixed liquid；
Step 3：The magnalium hydrotalcite powder obtained by step one is added into the dioxygen water mixed liquid described in step 2, it is whole to add
Enter process to be maintained under ice bath environment and be stirred continuously；
Step 4：Step 3 products therefrom is subjected to suction filtration, then with ethyl alcohol recrystallization twice, dried at room temperature, sealing is protected
Deposit；
Step 5：Water intaking, adds after ferrous salt or molysite, stirring and dissolving into water, step 4 products therefrom is added into water, whole
Individual process is kept stirring for, and the reaction time is 20 ~ 100 minutes；
Step 6：Step 5 products therefrom is subjected to suction filtration, after weak acid scrubbing 2 times, neutrality is washed with deionized, in
Room temperature ~ 100 DEG C are dried, sealing preserve.
2. the preparation method of arsenic-removing adsorption agent according to claim 2, it is characterised in that：Magnalium is prepared in the step one
Hydrotalcite powder specifically includes following steps：
Step（1）：Prepare the magnesium-aluminum metal mixed salt solution that molar concentration is 1 ~ 1.2 mol/L, the magnesium-aluminum metal salt mixing
The molar ratio range of magnesium and aluminium is 2 in solution:3~5:1；
Step（2）：Prepare the molar concentration of sodium carbonate in the mixed ammonium/alkali solutions that NaOH and sodium carbonate are constituted, mixed ammonium/alkali solutions
For 2 times of aluminium salt concentration in magnesium-aluminum metal mixed salt solution, the molar concentration of NaOH is in magnesium-aluminum metal mixed salt solution
1.6 times of metal ion total concentration；
Step（3）：Magnesium-aluminum metal mixed salt solution is instilled in deionized water with mixed ammonium/alkali solutions with identical constant drop speed, it is whole
Individual titration process is kept stirring for；
Step（4）：Continue to stir uniform to solution after the completion of titration, 3 ~ 24h is stood until solution crystallization at 60 ~ 180 DEG C；
Step（5）：The mixed liquor that crystallization is completed carries out suction filtration, and solid obtained by suction filtration is washed with deionized totally, then made
Use ethyl alcohol recrystallization；
Step（6）：The solid of recrystallization is dried, drying product is ground, magnalium hydrotalcite powder is obtained.
3. the preparation method of arsenic-removing adsorption agent according to claim 2, it is characterised in that：The step（1）In magnalium
Metal mixed salt solution is magnesium sulfate aluminium salt, magnesium nitrate aluminium salt, chlorine magnalium salt, one or more of combinations of magnesium carbonate aluminium salt.
4. the preparation method of arsenic-removing adsorption agent according to claim 3, it is characterised in that：What is added in the step 2 is steady
Agent is determined from magnesium sulfate, magnesium nitrate, sodium stannate, one kind of organic phosphate, and the proportion of stabilizer and hydrogen peroxide is
0.3:100~0.6:100。
5. the preparation method of arsenic-removing adsorption agent according to claim 4, it is characterised in that：Hydrogen peroxide in the step 3
It is more than 7 with the mass ratio of magnalium hydrotalcite powder.
6. the preparation method of arsenic-removing adsorption agent according to claim 5, it is characterised in that：Ferrous salt is selected in the step 5
With one kind of ferrous sulfate or frerrous chloride, molysite selects ferric sulfate, iron chloride, one kind of ferric nitrate.
7. the preparation method of arsenic-removing adsorption agent according to claim 6, it is characterised in that：Used in the step 6
Dilute acid concentration is less than 0.2 mol/L, and diluted acid is one kind of sulfuric acid, hydrochloric acid or nitric acid.
8. arsenic-removing adsorption agent made from the preparation method according to above-mentioned any one claim.
9. arsenic-removing adsorption agent made from the preparation method according to claim 1-7 pollutes answering for Adsorption in arsenic in water body
With.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710228854.9A CN106943984B (en) | 2017-04-10 | 2017-04-10 | A kind of arsenic-removing adsorption agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710228854.9A CN106943984B (en) | 2017-04-10 | 2017-04-10 | A kind of arsenic-removing adsorption agent and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106943984A true CN106943984A (en) | 2017-07-14 |
| CN106943984B CN106943984B (en) | 2019-05-21 |
Family
ID=59474329
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710228854.9A Expired - Fee Related CN106943984B (en) | 2017-04-10 | 2017-04-10 | A kind of arsenic-removing adsorption agent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106943984B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555554A (en) * | 2017-09-27 | 2018-01-09 | 大连理工大学 | A kind of capacitive deionization technology of oxygen-containing acid group using layered metal oxide arsenic-adsorbing |
| CN107638887A (en) * | 2017-09-22 | 2018-01-30 | 安徽大学 | A kind of C@NiFe LDH catalyst for Industrial Wastewater Treatment and preparation method thereof |
| CN108101158A (en) * | 2017-12-01 | 2018-06-01 | 常州大学 | A kind of method that material for water treatment is prepared using stalk |
| CN108404872A (en) * | 2018-05-29 | 2018-08-17 | 中国科学院生态环境研究中心 | Arsenic-removing adsorption agent and preparation method |
| CN108479689A (en) * | 2018-04-23 | 2018-09-04 | 中国环境科学研究院 | A kind of adsorbent of removal arsenic in waste water acid ion |
| CN108499516A (en) * | 2018-04-03 | 2018-09-07 | 中国神华能源股份有限公司 | Support type arsenic adsorbent and its preparation method and application and the method for arsenic removing |
| CN108579666A (en) * | 2018-05-14 | 2018-09-28 | 东南大学 | A method of preparing dearsenification adsorbent using spent bleaching clay |
| CN109692650A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | The adsorbent and preparation method thereof of arsenite ion in efficient removal water |
| CN111054358A (en) * | 2019-12-06 | 2020-04-24 | 西南石油大学 | Copper-nickel-tin hydrotalcite catalyst and preparation method thereof |
| CN112551746A (en) * | 2020-11-24 | 2021-03-26 | 衢州学院 | Treatment method of magnesium-containing wastewater in production process of organic silicon protective agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336461A (en) * | 2010-07-27 | 2012-02-01 | 中国科学院过程工程研究所 | Method for removing metal ions from aqueous solution by use of hydrotalcite |
| CN103127899A (en) * | 2011-11-29 | 2013-06-05 | 中国科学院烟台海岸带研究所 | Arsenic removal absorbent-iron and copper composite oxide and preparation method of copper composite oxide |
-
2017
- 2017-04-10 CN CN201710228854.9A patent/CN106943984B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336461A (en) * | 2010-07-27 | 2012-02-01 | 中国科学院过程工程研究所 | Method for removing metal ions from aqueous solution by use of hydrotalcite |
| CN103127899A (en) * | 2011-11-29 | 2013-06-05 | 中国科学院烟台海岸带研究所 | Arsenic removal absorbent-iron and copper composite oxide and preparation method of copper composite oxide |
Non-Patent Citations (1)
| Title |
|---|
| HOSSEIN ABDOLMOHAMMAD-ZADEH ET AL.: "Speciation of As(III)/As(V) in water samples by a magnetic solid phase extraction based on Fe3O4/Mg–Al layered double hydroxide nano-hybrid followed by chemiluminescence detection", 《TALANTA》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107638887B (en) * | 2017-09-22 | 2020-04-28 | 安徽大学 | C @ NiFe-LDH catalyst for industrial wastewater treatment and preparation method thereof |
| CN107638887A (en) * | 2017-09-22 | 2018-01-30 | 安徽大学 | A kind of C@NiFe LDH catalyst for Industrial Wastewater Treatment and preparation method thereof |
| CN107555554A (en) * | 2017-09-27 | 2018-01-09 | 大连理工大学 | A kind of capacitive deionization technology of oxygen-containing acid group using layered metal oxide arsenic-adsorbing |
| CN107555554B (en) * | 2017-09-27 | 2020-10-13 | 大连理工大学 | Capacitance deionization technology for absorbing oxyacid radical of arsenic by using layered metal oxide |
| CN109692650B (en) * | 2017-10-20 | 2022-07-08 | 中国石油化工股份有限公司 | Adsorbent for efficiently removing arsenite ions in water and preparation method thereof |
| CN109692650A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | The adsorbent and preparation method thereof of arsenite ion in efficient removal water |
| CN108101158A (en) * | 2017-12-01 | 2018-06-01 | 常州大学 | A kind of method that material for water treatment is prepared using stalk |
| CN108499516A (en) * | 2018-04-03 | 2018-09-07 | 中国神华能源股份有限公司 | Support type arsenic adsorbent and its preparation method and application and the method for arsenic removing |
| CN108479689A (en) * | 2018-04-23 | 2018-09-04 | 中国环境科学研究院 | A kind of adsorbent of removal arsenic in waste water acid ion |
| CN108579666A (en) * | 2018-05-14 | 2018-09-28 | 东南大学 | A method of preparing dearsenification adsorbent using spent bleaching clay |
| CN108404872A (en) * | 2018-05-29 | 2018-08-17 | 中国科学院生态环境研究中心 | Arsenic-removing adsorption agent and preparation method |
| CN111054358A (en) * | 2019-12-06 | 2020-04-24 | 西南石油大学 | Copper-nickel-tin hydrotalcite catalyst and preparation method thereof |
| CN111054358B (en) * | 2019-12-06 | 2022-02-01 | 西南石油大学 | Copper-nickel-tin hydrotalcite catalyst and preparation method thereof |
| CN112551746A (en) * | 2020-11-24 | 2021-03-26 | 衢州学院 | Treatment method of magnesium-containing wastewater in production process of organic silicon protective agent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106943984B (en) | 2019-05-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106943984B (en) | A kind of arsenic-removing adsorption agent and preparation method thereof | |
| CN104549127B (en) | Magnetic coupling hydroxyapatite nano particulate and its preparation method and application | |
| CN105363416A (en) | Manganese dioxide nanowire @ multidimensional mesoporous metal organic framework adsorbent and preparation method thereof | |
| CN105923628B (en) | Wastewater treatment method in graphene preparation process | |
| CN107051377B (en) | A kind of nanocomposite and preparation method thereof for synchronous removal carbon nitrogen phosphorus | |
| CN106334518B (en) | A kind of recyclable magnetic phosphorus adsorbent and preparation method thereof | |
| CN105536753B (en) | A kind of mineral precursor adsorbent and its preparation method and application | |
| CN103172119A (en) | Preparation method of layered chemical manganese dioxide | |
| JP5671437B2 (en) | Adsorbent manufacturing method | |
| CN104437539B (en) | A kind of magnetic OMS-2 catalyst and the application of degradable organic pollutant thereof | |
| CN113929492B (en) | Preparation method of hydrotalcite-like composite material for phosphorus recovery, product and application thereof | |
| CN104138750A (en) | Method for deep dephosphorization by using embedded lanthanum oxide composite resin | |
| CN102625777B (en) | The manufacture of electroplating sludge process and nano-level iron oxide compound | |
| CN104607228A (en) | Preparation method for alpha-Fe2O3 quantum dot/nitrogen-doped graphene composite material | |
| Ryu et al. | Mechanochemical synthesis of silica-lithium manganese oxide composite for the efficient recovery of lithium ions from seawater | |
| CN110743537B (en) | OMS-2 catalytic material and preparation method and application thereof | |
| CN106587120A (en) | Water treatment agent based on laminated composite metal hydroxide and preparation method of water treatment agent | |
| CN107686156B (en) | A kind of Fenton method of efficient degradation organic pollutants | |
| CN113600133A (en) | Phosphorus removal adsorbent and preparation method and application thereof | |
| CN104474662B (en) | Preparation method of stabilizer for treating arsenic-containing waste residue | |
| CN103769082A (en) | Preparation method of carbon-supported active MnOx, product of method and application of product | |
| CN111573770B (en) | Method for removing arsanilic acid in water by adopting ferromanganese oxide material | |
| CN111389360B (en) | Bio-carbon-loaded Ce-rich material3+Cerium dioxide material, preparation method and application thereof | |
| CN109126647A (en) | A kind of preparation method of graphene oxide-sodium alginate gel ball | |
| CN114733486B (en) | Preparation method of dephosphorization modified biochar |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190521 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |