CN108404880A - A kind of preparation method of inorganic dephosphorization adsorbent - Google Patents
A kind of preparation method of inorganic dephosphorization adsorbent Download PDFInfo
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- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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- 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
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- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- 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
- C02F2101/105—Phosphorus compounds
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Abstract
A kind of preparation method of inorganic dephosphorization adsorbent, belongs to technical field of absorbent.Specific preparation process is as follows:Weigh mesoporous silica molecular sieve drying;Mesopore molecular sieve after drying is added in ferric chloride solution, cerous nitrate solution and manganese sulfate solution, is stood after magnetic agitation;Mixed liquor filters after standing, and filter residue is put into Muffle kiln roasting, is ground after being cooled to room temperature;In fine powder after taking red mud, activated carbon, zirconium oxide and chitosan that grinding is added, deionized water is then added, adjusting pH with NaOH solution is more than 10, impregnates;Soak is filtered, dries under microwave, then grinds, be sealed.Preparation method raw material of the present invention is easy to get, preparation process is environmental-friendly, environmentally protective.The product phosphonium ion adsorption rate of preparation is high, large amount of adsorption and adsorption rate are fast.Inorganic dephosphorization adsorbent prepared by the present invention can adsorb totally 50mg/L phosphorus-containing wastewaters in 1 h, reach the standard for meeting discharge, adsorption rate is up to 95 ~ 98%.
Description
Technical field
The invention belongs to technical field of absorbent, and in particular to a kind of preparation method of inorganic dephosphorization adsorbent.
Background technology
The eutrophication of water body is one of the great environmental problem that current countries in the world are faced, and phosphorus is to cause water body rich
The key nutriment of nutrient laden.Therefore, for conservation of nature water body environment, body eutrophication is prevented, people are increasingly
Pay close attention to the phosphorus ligands of phosphorous industrial wastewater and sanitary sewage.Currently, multiple technologies have been used to the removal of phosphorus, such as bioanalysis is changed
Learn Coagulation Method, ion-exchange, membrane separation process, artificial swamp method, electrochemical process, absorption method etc..Wherein, absorption method is considered having
There is preferable application prospect, since it has many advantages, such as efficient, economic, easy to operate and non-secondary pollution, according to the literature, commonly uses
Phosphorus adsorbent have goethite, flyash, diatomite, iron aluminium composite oxide, ferrozirconium composite oxides, rare earth oxide, manganese
Oxide etc..But existing dephosphorization adsorbent function and effect are slow, adsorbance is small, it is also necessary to be improved again.
Invention content
The technical issues of solution:In view of the above technical problems, the present invention provides a kind of preparation side of inorganic dephosphorization adsorbent
Method has the high product phosphonium ion adsorption rate that raw material is easy to get, preparation process is environmental-friendly, prepares, large amount of adsorption and adsorbs speed
Spend the advantages that fast.
Technical solution:A kind of preparation method of inorganic dephosphorization adsorbent, the preparation method comprises the following steps:
Step 1 weighs 2~6 mass parts mesoporous silica molecular sieves dry 6~8h at a temperature of 90~120 DEG C;
20~30 mass parts 1.5mol/L ferric chloride solutions, 10~15 matter are added in mesopore molecular sieve after step 2 will be dried
It measures in part 0.8mol/L cerous nitrate solutions and 15~35 mass parts 1mol/L manganese sulfate solutions, it is quiet after 30~45min of magnetic agitation
Set 4~6h;
Mixed liquor filters after step 3 will be stood, and filter residue is put into Muffle furnace and roasts 1~2h for 140~155 DEG C, then cold
But to being ground after room temperature, 80~120 mesh sieve is crossed;
Step 4 weighs 2~4 mass parts red muds, 1~3 mass parts activated carbon, 0.5~0.8 mass parts zirconium oxide and 2~4
Mass parts chitosan is added in the fine powder after step 3 grinding, 40~50 mass parts deionized waters is then added, with 5mol/L's
NaOH solution adjusts pH and is more than 10, impregnates 2~4h;
Step 5 filters soak, and 6~10min is dried at 200~400W of microwave power, is then ground, excessively 200~
300 mesh sieve, and are sealed.
Preferably, the model MCM41 of mesopore molecular sieve described in the step 1.
Preferably, weighing 4 mass parts mesoporous silica molecular sieves dry 7h at a temperature of 100 DEG C in the step 1.
Preferably, mesopore molecular sieve 25 mass parts 1.5mol/L iron chloride of addition are molten after will be dry in the step 2
In liquid, 12 mass parts 0.8mol/L cerous nitrate solutions and 20 mass parts 1mol/L manganese sulfate solutions, stood after magnetic agitation 40min
5h。
Preferably, mixed liquor filters after being stood in the step 3, filter residue is put into 150 DEG C of roastings in Muffle furnace
1.5h is ground after then cooling to room temperature, sieves with 100 mesh sieve.
Preferably, weighing 3 mass parts red muds, 2 mass parts activated carbons, 0.6 mass parts zirconium oxide and 3 in the step 4
Mass parts chitosan is added in the fine powder after step 3 grinding, 45 mass parts deionized waters is then added, with the NaOH of 5mol/L
Solution adjusts pH and is more than 10, impregnates 3h.
Preferably, filtering soak in the step 5,8min is dried at microwave power 300W, is then ground, mistake
250 mesh sieve, and are sealed.
Advantageous effect:Preparation method raw material of the present invention is easy to get, preparation process is environmental-friendly, environmentally protective.It prepares
Product phosphonium ion adsorption rate height, large amount of adsorption and adsorption rate are fast.By carrying out magnetic modification to mesopore molecular sieve, then in conjunction with
Zirconium oxide is modified the synergistic function of mesoporous silica molecular sieve with red mud, activated carbon, chitosan, magnetic, and the present invention is prepared inorganic
Dephosphorization adsorbent can adsorb totally 50mg/L phosphorus-containing wastewaters in 1h, reach the standard for meeting discharge, adsorption rate is up to 95
~98%.
Specific implementation mode
Embodiment 1
A kind of preparation method of inorganic dephosphorization adsorbent, the preparation method comprises the following steps:
Step 1 weighs 2 mass parts mesoporous silica molecular sieves dry 6h, model of the mesopore molecular sieve at a temperature of 90 DEG C
For MCM41.
20 mass parts 1.5mol/L ferric chloride solutions, 10 mass parts are added in mesopore molecular sieve after step 2 will be dried
In 0.8mol/L cerous nitrate solutions and 15 mass parts 1mol/L manganese sulfate solutions, 4h is stood after magnetic agitation 30min.
Mixed liquor filters after step 3 will be stood, and filter residue is put into 140 DEG C of roasting 1h in Muffle furnace, then cools to room temperature
After be ground, cross 80 mesh sieve.
Step 4 weighs 2 mass parts red muds, 1 mass parts activated carbon, 0.5 mass parts zirconium oxide and 2 mass parts chitosans and adds
Enter in the fine powder after step 3 grinding, 40 mass parts deionized waters are then added, adjusting pH with the NaOH solution of 5mol/L is more than
10, impregnate 2h.
Step 5 filters soak, and 6min is dried at microwave power 200W, is then ground, and crosses 200 mesh sieve, and sealing is protected
It deposits.
Embodiment 2
A kind of preparation method of inorganic dephosphorization adsorbent, the preparation method comprises the following steps:
Step 1 weighs 6 mass parts mesoporous silica molecular sieves dry 8h, type of the mesopore molecular sieve at a temperature of 120 DEG C
Number be MCM41.
30 mass parts 1.5mol/L ferric chloride solutions, 15 mass parts are added in mesopore molecular sieve after step 2 will be dried
In 0.8mol/L cerous nitrate solutions and 35 mass parts 1mol/L manganese sulfate solutions, 6h is stood after magnetic agitation 45min.
Mixed liquor filters after step 3 will be stood, and filter residue is put into 155 DEG C of roasting 2h in Muffle furnace, then cools to room temperature
After be ground, cross 120 mesh sieve.
Step 4 weighs 4 mass parts red muds, 3 mass parts activated carbons, 0.8 mass parts zirconium oxide and 4 mass parts chitosans and adds
Enter in the fine powder after step 3 grinding, 50 mass parts deionized waters are then added, adjusting pH with the NaOH solution of 5mol/L is more than
10, impregnate 4h.
Step 5 filters soak, and 10min is dried at microwave power 400W, is then ground, and crosses 300 mesh sieve, and sealing is protected
It deposits.
Embodiment 3
A kind of preparation method of inorganic dephosphorization adsorbent, the preparation method comprises the following steps:
Step 1 weighs 4 mass parts mesoporous silica molecular sieves dry 7h, type of the mesopore molecular sieve at a temperature of 100 DEG C
Number be MCM41.
25 mass parts 1.5mol/L ferric chloride solutions, 12 mass parts are added in mesopore molecular sieve after step 2 will be dried
In 0.8mol/L cerous nitrate solutions and 20 mass parts 1mol/L manganese sulfate solutions, 5h is stood after magnetic agitation 40min.
Mixed liquor filters after step 3 will be stood, and filter residue is put into 150 DEG C of roasting 1.5h in Muffle furnace, is subsequently cooled to room
It is ground, sieves with 100 mesh sieve after temperature.
Step 4 weighs 3 mass parts red muds, 2 mass parts activated carbons, 0.6 mass parts zirconium oxide and 3 mass parts chitosans and adds
Enter in the fine powder after step 3 grinding, 45 mass parts deionized waters are then added, adjusting pH with the NaOH solution of 5mol/L is more than
10, impregnate 3h.
Step 5 filters soak, and 8min is dried at microwave power 300W, is then ground, and crosses 250 mesh sieve, and sealing is protected
It deposits.
Comparative example 1
With embodiment 3, difference lies in do not add zirconium oxide, specific preparation process is as follows:
Step 1 weighs 4 mass parts mesoporous silica molecular sieves dry 7h, type of the mesopore molecular sieve at a temperature of 100 DEG C
Number be MCM41.
25 mass parts 1.5mol/L ferric chloride solutions, 12 mass parts are added in mesopore molecular sieve after step 2 will be dried
In 0.8mol/L cerous nitrate solutions and 20 mass parts 1mol/L manganese sulfate solutions, 5h is stood after magnetic agitation 40min.
Mixed liquor filters after step 3 will be stood, and filter residue is put into 150 DEG C of roasting 1.5h in Muffle furnace, is subsequently cooled to room
It is ground, sieves with 100 mesh sieve after temperature.
After step 4 weighs 3 mass parts red muds, 2 mass parts activated carbons and the addition step 3 grinding of 3 mass parts chitosans
In fine powder, 45 mass parts deionized waters are then added, adjusting pH with the NaOH solution of 5mol/L is more than 10, impregnates 3h.
Step 5 filters soak, and 8min is dried at microwave power 300W, is then ground, and crosses 250 mesh sieve, and sealing is protected
It deposits.
Phosphorous (in terms of the P elements) aqueous solution of 50mg/L is prepared with deionized water.In 250mL conical flasks, it is added
100mL phosphorus solutions, with NaOH and HCl come adjust solution ph be 5.6, accurately weigh and 0.2g Examples 1 to 3 and comparison be added
Absorbent powder prepared by example 1, mixed liquor is shaken under the conditions of 25 DEG C, 150r/min and is shaken up, and the anti-light splitting light of molybdenum antimony is used after 1h
Degree method measures phosphorus concentration, and adsorbance is calculated as follows:
Q in formulaeIt is equilibrium adsorption capacity, mg/g;c0It is the initial concentration of solution, mg/L;ceBe absorption after solution balance it is dense
Degree, mg/L;V is the volume of solution, L;M is the quality that adsorbent is added, g.
Dephosphorizing rate η (%) calculation formula is as follows:
Test result is as follows for product dephosphorizing rate prepared by Examples 1 to 3 and comparative example 1:
Dephosphorizing rate/% | |
Embodiment 1 | 95 |
Embodiment 2 | 97 |
Embodiment 3 | 98 |
Comparative example 1 | 89 |
Claims (7)
1. a kind of preparation method of inorganic dephosphorization adsorbent, which is characterized in that the preparation method comprises the following steps:
Step 1 weighs 2 ~ 6 mass parts mesoporous silica molecular sieves dry 6 ~ 8 h at a temperature of 90 ~ 120 DEG C;
20 ~ 30 mass parts, 1.5 mol/L ferric chloride solutions, 10 ~ 15 mass parts are added in mesopore molecular sieve after step 2 will be dried
In 1 mol/L manganese sulfate solutions of 0.8 mol/L cerous nitrate solutions and 15 ~ 35 mass parts, after 30 ~ 45 min of magnetic agitation stand 4 ~
6 h;
Mixed liquor filters after step 3 will be stood, and filter residue is put into 140 ~ 155 DEG C of 1 ~ 2 h of roasting in Muffle furnace, is subsequently cooled to room
It is ground after temperature, crosses 80 ~ 120 mesh sieve;
Step 4 weighs 2 ~ 4 mass parts red muds, 1 ~ 3 mass parts activated carbon, 0.5 ~ 0.8 mass parts zirconium oxide and 2 ~ 4 mass parts shells
Glycan is added in the fine powder after step 3 grinding, 40 ~ 50 mass parts deionized waters is then added, with the NaOH solution of 5 mol/L
It adjusts pH and is more than 10, impregnate 2 ~ 4 h;
Step 5 filters soak, and 6 ~ 10 min are dried at 200 ~ 400W of microwave power, are then ground, and crosses 200 ~ 300 mesh
Sieve, is sealed.
2. a kind of preparation method of inorganic dephosphorization adsorbent according to claim 1, which is characterized in that in the step 1
The model MCM41 of the mesopore molecular sieve.
3. a kind of preparation method of inorganic dephosphorization adsorbent according to claim 1, which is characterized in that in the step 1
Weigh 4 mass parts mesoporous silica molecular sieves dry 7 h at a temperature of 100 DEG C.
4. a kind of preparation method of inorganic dephosphorization adsorbent according to claim 1, which is characterized in that in the step 2
It is molten that 25 mass parts, 1.5 mol/L ferric chloride solutions, 12 mass parts, 0.8 mol/L cerous nitrates is added in mesopore molecular sieve after will be dry
In 1 mol/L manganese sulfate solutions of liquid and 20 mass parts, 5 h are stood after 40 min of magnetic agitation.
5. a kind of preparation method of inorganic dephosphorization adsorbent according to claim 1, which is characterized in that in the step 3
Mixed liquor filters after standing, and filter residue is put into 150 DEG C of 1.5 h of roasting in Muffle furnace, is ground after then cooling to room temperature, mistake
100 mesh sieve.
6. a kind of preparation method of inorganic dephosphorization adsorbent according to claim 1, which is characterized in that in the step 4
After weighing 3 mass parts red muds, 2 mass parts activated carbons, 0.6 mass parts zirconium oxide and the addition step 3 grinding of 3 mass parts chitosans
Fine powder in, 45 mass parts deionized waters are then added, adjusting pH with the NaOH solution of 5 mol/L is more than 10, impregnates 3 h.
7. a kind of preparation method of inorganic dephosphorization adsorbent according to claim 1, which is characterized in that in the step 5
Soak is filtered, 8 min are dried at microwave power 300W, are then ground, 250 mesh sieve is crossed, is sealed.
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Cited By (4)
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CN110694585A (en) * | 2019-09-23 | 2020-01-17 | 北京工业大学 | Preparation method of zirconium modified red mud phosphorus removal adsorbent |
CN111039658A (en) * | 2019-12-31 | 2020-04-21 | 广东省水利水电科学研究院 | Phosphorus removal ceramsite and preparation method thereof |
CN112973635A (en) * | 2021-03-23 | 2021-06-18 | 江苏嘉盛旺环境科技有限公司 | Preparation process of sewage dephosphorization activated carbon |
CN116282339A (en) * | 2023-05-09 | 2023-06-23 | 佛山科学技术学院 | Groundwater treatment method |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110694585A (en) * | 2019-09-23 | 2020-01-17 | 北京工业大学 | Preparation method of zirconium modified red mud phosphorus removal adsorbent |
CN111039658A (en) * | 2019-12-31 | 2020-04-21 | 广东省水利水电科学研究院 | Phosphorus removal ceramsite and preparation method thereof |
CN112973635A (en) * | 2021-03-23 | 2021-06-18 | 江苏嘉盛旺环境科技有限公司 | Preparation process of sewage dephosphorization activated carbon |
CN112973635B (en) * | 2021-03-23 | 2023-08-18 | 江苏嘉盛旺环境科技有限公司 | Preparation process of sewage dephosphorization activated carbon |
CN116282339A (en) * | 2023-05-09 | 2023-06-23 | 佛山科学技术学院 | Groundwater treatment method |
CN116282339B (en) * | 2023-05-09 | 2023-09-26 | 佛山科学技术学院 | Groundwater treatment method |
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