CN107698009A - A kind of carbon containing magnesium salts material for removing removing heavy metals and its preparation method and application - Google Patents
A kind of carbon containing magnesium salts material for removing removing heavy metals and its preparation method and application Download PDFInfo
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- CN107698009A CN107698009A CN201710981522.8A CN201710981522A CN107698009A CN 107698009 A CN107698009 A CN 107698009A CN 201710981522 A CN201710981522 A CN 201710981522A CN 107698009 A CN107698009 A CN 107698009A
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- magnesium salts
- carbon containing
- containing magnesium
- salts material
- heavy metals
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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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
A kind of carbon containing magnesium salts material for removing removing heavy metals and its preparation method and application, MgO and methanol are mixed under ultrasound first, phosphoric acid is added dropwise afterwards, then moves to water heating kettle insulation, centrifuged after reaction product is cleaned and be dried to obtain solid, solid is ground to obtain dusty material.The present invention is prepared for carbon containing magnesium salts material by solvent-thermal method, can rapidly remove the heavy metal including Cd, Pb in water, and clearance can control content of beary metal in drinking water standard up to more than 99%, have extraordinary purifying water effect and application potential.
Description
Technical field
The present invention relates to water purification field, and in particular to a kind of carbon containing magnesium salts material that effectively can quickly remove heavy metal in water removal
And its preparation method and application.
Background technology
Pollution of the heavy metals such as Cd, Pb caused by industrial production in water body has seriously endangered health.Mesh
Preceding plant chimney stalk mainly handles heel row by chemical precipitation method, oxidation-reduction method, membrane separation technique and the method for biological treatment
Put.In the various methods of water process, not up to standard, inorganic agent preparation technology after long the time required to processing being present, heavy metal processing
Complicated and introducing secondary pollution problems.Therefore need to invent a kind of fast and effective material for removing removing heavy metals of energy popularization and application
Preparation method.
The content of the invention
The technical problem of solution：The problem of present invention is prepared for the effective removal heavy metal material faced instantly, there is provided
A kind of carbon containing magnesium salts material for removing removing heavy metals and its preparation method and application.
Technical scheme：A kind of preparation method for the carbon containing magnesium salts material for removing removing heavy metals, including following preparation process：Step
（1）：MgO powder and methanol are sufficiently mixed under ultrasound, obtain mixing turbid, per 1L methanol in MgO additions 20-60 g it
Between, 15-75 DEG C of ultrasonic temperature, ultrasonic mixing time 0.5-1 h；Step（2）：By step（1）Gained mixing turbid moves into hydro-thermal
Phosphoric acid is added dropwise after reactor, is thoroughly mixed, often adjusts 1L methanol phosphoric acid 0-60 mL；Step（3）：Will step
Suddenly（2）Middle reactor is placed in baking oven heating, and the 50-140 DEG C of h of freeze-day with constant temperature 4 obtains non-newtonian fluid；Step（4）：By step（3）
Non-newtonian fluid after processing is stirred, then will wash clean carbon containing magnesium salts material after the centrifugation of obtained turbid；Step
（5）：By step（4）Carbon containing magnesium salts material after processing carries out 70-85 DEG C of drying process and is incubated, then grinds and produce carbon containing magnesium
Salt material.
Preferably, per 50mL methanol in MgO additions be 1.2786g, 50 DEG C of ultrasonic temperature, the h of ultrasonic mixing time 0.5
Preferably, mix and phosphoric acid is added in turbid, regulation 50mL methanol phosphatase 11 .5mL.
Preferably, 110 DEG C of baking oven heating-up temperature is adjusted, is cooled down at room temperature after the h of heated at constant temperature 4.
Preferably, 80 DEG C of drying temperature and it is incubated.
The carbon containing magnesium salts material that the above method is prepared.
Application of the above-mentioned carbon containing magnesium salts material in removing heavy metals are removed.
Beneficial effect：The present invention by solvent-thermal method is prepared for carbon containing magnesium salts material, at high temperature under high pressure, phosphoric acid by with
Magnesia and the intermediate product of alcohol reaction generation（HOMgOCH3）Further reaction is formed rich in carbonate, the magnesium salts material of phosphate radical
Material；In addition, the volatilization of alcohol forms porous on magnesium salts surface during drying, specific surface area is increased.Test result shows the material pair
The clearance of the heavy metals such as Pb, Cd can reach more than 99%, and Pb, Cd content can be limited to content of beary metal mark in drinking water
Standard, go removing heavy metals required time that there is extraordinary application prospect within 2 h.
Brief description of the drawings
Fig. 1 is the Pb residual concentrations measured under identical phosphorus content, different temperatures；
Fig. 2 is the Cd residual concentrations measured under identical phosphorus content, different temperatures；
Fig. 3 is the Pb residual concentrations measured under mutually synthermal, different phosphorus contents；
Fig. 4 is the Cd residual concentrations measured under mutually synthermal, different phosphorus contents；
Fig. 5 is that the carbon containing magnesium salts that have selected at 110 DEG C shown in embodiment 5 is gone with commercial magnesia in the amount of being excessively added situation
Except Pb dynamic curve diagram.
Embodiment
The invention will be further elaborated by the following examples.The present embodiment is premised on technical solution of the present invention
Under implemented, give detailed embodiment and process, but the scope of the present invention is not limited to following embodiments.Under
Unreceipted condition and method etc. are carried out according to the condition proposed by routine or manufacturer in the embodiment in face.Lead to below
Cross the carbon containing magnesium salts material that specific implementation method prepares solvent-thermal method to be explained in detail, temperature is reacted in reactor by adjusting
Degree and phosphorus acid content obtain.
Embodiment 1
Step（1）：1.2786 g MgO powder and 50 mL methanol are sufficiently mixed 30 min under 50 DEG C of ultrasound；
Step（2）：By step（1）1.5 mL phosphoric acid are added dropwise after moving into hydrothermal reaction kettle in mixed turbid, carry out abundant
It is stirred；
Step（3）：By step（2）It is middle to complete mixed reactor and be placed in baking oven to heat 4 h, regulation temperature is respectively 50 DEG C,
80 ℃、110 ℃、140 ℃；
Step（4）：By step（3）Non-newtonian fluid after processing is stirred, then washes 3-5 after obtained turbid is centrifuged
Time；
Step（5）：By step（4）Carbon containing magnesium salts material drying process at 80 DEG C after processing, powder is can obtain after grinding
The carbon containing magnesium salts material of shape.
The mL of raw water containing Pb 250 that initial concentration is about 10 mg/L is prepared, the water purification material 0.25 g is added, in magnetic force
Lower 2 h of stirring, detection Pb concentration is sampled with syringe filters.Pb residual concentrations under different temperatures are shown in Fig. 1.
Embodiment 2
Step（1）：1.2786 g MgO powder and 50 mL methanol are sufficiently mixed 30 min under 50 DEG C of ultrasound；
Step（2）：By step（1）1.5 mL phosphoric acid are added dropwise after moving into hydrothermal reaction kettle in mixed turbid, carry out abundant
It is stirred；
Step（3）：By step（2）It is middle to complete mixed reactor and be placed in baking oven to heat 4 h, regulation temperature is respectively 50 DEG C,
80 ℃、110 ℃、140 ℃；
Step（4）：By step（3）Non-newtonian fluid after processing is stirred, then washes 3-5 after obtained turbid is centrifuged
Time；
Step（5）：By step（4）Carbon containing magnesium salts material drying process at 80 DEG C after processing, powder is can obtain after grinding
The carbon containing magnesium salts material of shape.
The mL of raw water containing Cd 250 that initial concentration is about 6 mg/L is prepared, the water purification material 0.25 g is added, in magnetic force
Lower 2 h of stirring, detection Cd concentration is sampled with syringe filters.Cd residual concentrations under different temperatures are shown in Fig. 2.
Embodiment 3
Step（1）：1.2786 g MgO powder and 50 mL methanol are sufficiently mixed 30 min under 50 DEG C of ultrasound；
Step（2）：By step（1）Phosphoric acid is added dropwise after moving into hydrothermal reaction kettle in mixed turbid, be sufficiently stirred mixed
Close, regulation phosphorus acid content is respectively 0.5 mL, 1.0 mL, 1.5 mL, 2.5 mL；
Step（3）：By step（2）The middle mixed reactor of completion is placed in baking oven and heats 4 h, and regulation temperature is respectively 110
℃；
Step（4）：By step（3）Non-newtonian fluid after processing is stirred, then washes 3-5 after obtained turbid is centrifuged
Time；
Step（5）：By step（4）Carbon containing magnesium salts material drying process at 80 DEG C after processing, powder is can obtain after grinding
The carbon containing magnesium salts material of shape.
The mL of raw water containing Pb 250 that initial concentration is about 10 mg/L is prepared, the water purification material 0.25 g is added, in magnetic force
Lower 2 h of stirring, detection Pb concentration is sampled with syringe filters.Pb residual concentrations under different temperatures are shown in Fig. 3.
Embodiment 4
Step（1）：1.2786 g MgO powder and 50 mL methanol are sufficiently mixed 30 min under 50 DEG C of ultrasound；
Step（2）：By step（1）Phosphoric acid is added dropwise after moving into hydrothermal reaction kettle in mixed turbid, be sufficiently stirred mixed
Close, regulation phosphorus acid content is respectively 0.5 mL, 1.0 mL, 1.5 mL, 2.5 mL；
Step（3）：By step（2）The middle mixed reactor of completion is placed in baking oven and heats 4 h, and regulation temperature is respectively 110
℃；
Step（4）：By step（3）Non-newtonian fluid after processing is stirred, then washes 3-5 after obtained turbid is centrifuged
Time；
Step（5）：By step（4）Carbon containing magnesium salts material drying process at 80 DEG C after processing, powder is can obtain after grinding
The carbon containing magnesium salts material of shape.
The mL of raw water containing Cd 250 that initial concentration is about 6 mg/L is prepared, the water purification material 0.25 g is added, in magnetic force
Lower 2 h of stirring, detection Cd concentration is sampled with syringe filters.Cd residual concentrations under different temperatures are shown in Fig. 4.
Embodiment 5
Step（1）：1.2786 g MgO powder and 50 mL methanol are sufficiently mixed 30 min under 50 DEG C of ultrasound；
Step（2）：By step（1）1.5 mL phosphoric acid are added dropwise after moving into hydrothermal reaction kettle in mixed turbid, carry out abundant
It is stirred；
Step（3）：By step（2）The middle mixed reactor of completion is placed in baking oven and heats 4 h, and regulation temperature is 110 DEG C；
Step（4）：By step（3）Non-newtonian fluid after processing is stirred, then is washed 3 times after obtained turbid is centrifuged；
Step（5）：By step（4）Carbon containing magnesium salts material drying process at 80 DEG C after processing, powder is can obtain after grinding
The carbon containing magnesium salts material of shape.
The low concentration Pb raw water solution of two glasss of same concentrations is prepared, the water purification material is separately added into and commercial magnesia is each
0.25 g, sample detection Pb concentration with syringe filters every a period of time under magnetic stirring.The excessive lower Pb of remover addition is residual
The kinetic curve of rate is stayed to see Fig. 5.
It should be noted that above for the exemplary work of the present invention, the feature in the range of patent requirements of the present invention can be entered
The arbitrary change of row, combination.
Claims (7)
1. a kind of preparation method for the carbon containing magnesium salts material for removing removing heavy metals, it is characterised in that including following preparation process：
Step（1）：MgO powder and methanol are sufficiently mixed under ultrasound, obtain mixing turbid, MgO additions exist in every 1L methanol
Between 20-60 g, 15-75 DEG C of ultrasonic temperature, ultrasonic mixing time 0.5-1 h；
Step（2）：By step（1）Phosphoric acid is added dropwise after moving into hydrothermal reaction kettle in gained mixing turbid, be sufficiently stirred mixed
Close, often adjust 1L methanol phosphoric acid 0-60 mL；
Step（3）：By step（2）Middle reactor is placed in baking oven heating, and the 50-140 DEG C of h of freeze-day with constant temperature 4 obtains non-newtonian fluid；
Step（4）：By step（3）Non-newtonian fluid after processing is stirred, then is washed after obtained turbid is centrifuged clean
Obtain carbon containing magnesium salts material；
Step（5）：By step（4）Carbon containing magnesium salts material after processing carries out 70-85 DEG C of drying process and is incubated, then grinds i.e.
Obtain carbon containing magnesium salts material.
A kind of 2. preparation method for the carbon containing magnesium salts material for removing removing heavy metals according to claim 1, it is characterised in that 50mL
MgO additions are 1.2786g in methanol, 50 DEG C of ultrasonic temperature, the h of ultrasonic mixing time 0.5.
A kind of 3. preparation method for the carbon containing magnesium salts material for removing removing heavy metals according to claim 1, it is characterised in that mixing
Phosphoric acid, regulation 50mL methanol phosphatase 11 .5mL are added in turbid.
A kind of 4. preparation method for the carbon containing magnesium salts material for removing removing heavy metals according to claim 1, it is characterised in that regulation
110 DEG C of baking oven heating-up temperature, cool down at room temperature after the h of heated at constant temperature 4.
5. a kind of preparation method for the carbon containing magnesium salts material for removing removing heavy metals according to claim 1, it is characterised in that dry
80 DEG C of temperature is simultaneously incubated.
6. the carbon containing magnesium salts material that any methods described of claim 1 ~ 5 is prepared.
7. application of the carbon containing magnesium salts material in removing heavy metals are removed described in claim 6.
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| CN201710981522.8A CN107698009B (en) | 2017-10-20 | 2017-10-20 | Carbon-containing magnesium salt material for removing heavy metals, and preparation method and application thereof |
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| CN107698009B CN107698009B (en) | 2021-03-02 |
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Citations (7)
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|---|---|---|---|---|
| CN101391783A (en) * | 2008-11-18 | 2009-03-25 | 天津工业大学 | Microemulsion solvent thermal synthesizing method of magnesium carbonate hollow and nano stick |
| KR20140002166A (en) * | 2012-06-28 | 2014-01-08 | 한국과학기술연구원 | Alginate complex impregnated magnesium compound, preparation method of the same and method for removal of heavy metals using the same |
| CN105195103A (en) * | 2015-07-06 | 2015-12-30 | 河北工业大学 | Carbon material for adsorbing heavy metal ions in water and application of carbon material |
| WO2016042321A1 (en) * | 2014-09-15 | 2016-03-24 | University Of York | Mesoporous materials from nanoparticle enhanced polysaccharides |
| CN105858832A (en) * | 2016-04-12 | 2016-08-17 | 合肥工业大学 | Heavy metal wastewater treatment material and method thereof |
| CN106345417A (en) * | 2016-11-03 | 2017-01-25 | 张静 | Method for preparing material for removing and adsorbing heavy metal lead in wastewater |
| CN107161970A (en) * | 2017-07-03 | 2017-09-15 | 南京纳铠生物医药科技有限公司 | It is a kind of that there is magnesium phosphate nano material of flourishing mesopore orbit structure and preparation method thereof |
-
2017
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391783A (en) * | 2008-11-18 | 2009-03-25 | 天津工业大学 | Microemulsion solvent thermal synthesizing method of magnesium carbonate hollow and nano stick |
| KR20140002166A (en) * | 2012-06-28 | 2014-01-08 | 한국과학기술연구원 | Alginate complex impregnated magnesium compound, preparation method of the same and method for removal of heavy metals using the same |
| WO2016042321A1 (en) * | 2014-09-15 | 2016-03-24 | University Of York | Mesoporous materials from nanoparticle enhanced polysaccharides |
| CN105195103A (en) * | 2015-07-06 | 2015-12-30 | 河北工业大学 | Carbon material for adsorbing heavy metal ions in water and application of carbon material |
| CN105858832A (en) * | 2016-04-12 | 2016-08-17 | 合肥工业大学 | Heavy metal wastewater treatment material and method thereof |
| CN106345417A (en) * | 2016-11-03 | 2017-01-25 | 张静 | Method for preparing material for removing and adsorbing heavy metal lead in wastewater |
| CN107161970A (en) * | 2017-07-03 | 2017-09-15 | 南京纳铠生物医药科技有限公司 | It is a kind of that there is magnesium phosphate nano material of flourishing mesopore orbit structure and preparation method thereof |
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| JOHAN FORSGREN等: "A Template-Free, Ultra-Adsorbing, High Surface Area Carbonate Nanostructure", 《PLOS ONE》 * |
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