CN104971691A - Nanometer magnesium silicate adsorbing material and preparation method therefor - Google Patents
Nanometer magnesium silicate adsorbing material and preparation method therefor Download PDFInfo
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Abstract
The invention provides a method for preparing an efficient nanometer magnesium silicate adsorbing material by using common raw materials through simple steps. A magnesium silicate colloid is synthesized by a liquid film reactor and a nucleation-crystallizing isolating method, and nanometer magnesium silicate particles are obtained through low temperature drying. The rotating liquid film reactor is used, and reaction conditions are regulated, so that the agglomeration of products is effectively improved, and the particle diameter of the products is decreased. Tests prove that the prepared magnesium silicate adsorbing material is the particles of 100nm-2 <mu>m, the specific surface area is 140-200m2/g, and the magnesium silicate adsorbing material has excellent characteristics of rich hole structures, large specific surface area, high surface charge and the like. The capacity of the magnesium silicate adsorbing material for removing organic dye namely methylene blue is excellent, after about 10 minutes, an adsorption reaction is close to balance, and under the premise that the removing rate is ensured to be more than 90%, the largest adsorption quantity achieves 280-365mg/g. The preparation method provided by the invention has high maneuverability, the used raw materials are cheap, the industrial production is facilitated, and the preparation method has wide application prospects in the field of wastewater treatment.
Description
Technical field:
The invention belongs to inorganic functional material preparing technical field, be specifically related to a kind of nanometer magnesium silicate sorbing material and preparation method thereof.
Background technology:
Water pollutions is one of bottleneck problem of running into of current social development, and harmful organic dyestuff of industrial discharge and toxic heavy metal ion are the important pollution sources of current water pollutions, directly threatens the productive life of the mankind and healthy.Developing efficient and feasible sewage disposal technology is society significant problem urgently to be resolved hurrily.
Current sewage disposal technology mainly contains physical method, biological method and chemical method.Wherein, physisorphtion is the most frequently used is also a kind of most economical method.The core of the method develops efficiently and the sorbing material of cheapness.At the sorbing material studied at present as in natural zeolite, active carbon etc., magnesium silicate, because of the layer structure of its uniqueness, special surface charge adsorption property and the strong selectivity to positive charge contaminated ion, causes the extensive concern of people.
Particle diameter is little and finely dispersed magnesium silicate material will have more adsorption site, is conducive to the performance of performance, and the synthesis condition of these parameters and magnesium silicate material and method closely bound up.
Document (Y Wang, G Wang, H Wang, C Liang, W Cai, L Zhang, Chem.Eur.J.2010,16,3497-3503) with nano silicon bead for template, prepared magnesium silicate hollow Nano bead that is diameter about 500nm, uniform, band whisker by hard template method, its to methylene blue be adsorbed on 10min within arrive balance, and maximal absorptive capacity reaches 207mg/g.But the method needs first to prepare mono-dispersed nano silica gel bead, then as templated synthesis magnesium silicate, harsh to the requirement of raw material and preparation condition, be not easy to large-scale production.
Document (Feng Ling, Li Min, Liu Guoqiang, Han Lei, Yang Ru, Beijing University of Chemical Technology journal .2010,37,70-75) with sodium metasilicate and magnesium nitrate for raw material, adopt the precipitation method to obtain adsorption of magnesium silicate material, it only has about 100mg/g to the most high adsorption capacity of methylene blue.Document (Chen Shuying, Sichuan chemical industry and corrosion control .2000,3,3-6) is with sodium metasilicate and magnesium chloride for raw material has prepared adsorption of magnesium silicate material, and it is only 114mg/g to the adsorption capacity of methylene blue.Document (F.Ferrero, Journal of EnvironmentalSciences 2010,22,467 – 473) use the adsorption of magnesium silicate material buied from U.S.Silica Company to process methylene blue solution, even if when experiment shows the concentration of Methylene Blue in Solution up to 1000mg/L, after 360min, it also only has 98mg/g to the adsorbance of methylene blue.The particle diameter of the magnesium silicate material that above-mentioned document uses is all millimeter or micron dimension, causes its external surface area less, is not easy to fully contact with adsorbate, limits the performance of materials adsorption performance.
Thus how attract attention with the adsorption of magnesium silicate material that raw material cheap and easy to get and method simple to operation prepare small particle diameter.
Summary of the invention:
The object of the present invention is to provide a kind of nanometer magnesium silicate sorbing material and the preparation method of this material is provided.This preparation method has very strong operability, and its obtained nanometer magnesium silicate sorbing material has excellent absorption property, can be used as the adsorbent of dye wastewater treatment.
The present invention with sodium metasilicate and magnesium salts for raw material, utilize rotating liquid-film reactor can moment fast nucleation feature, make sodium metasilicate and magnesium salts even fast nucleation in rotating liquid-film reactor, prepare small particle diameter magnesium silicate nucleus, more namely nucleus crystallization within the scope of 120 ~ 190 DEG C is obtained adsorption of magnesium silicate material.
The chemical general formula of nanometer magnesium silicate provided by the invention is: Mg
xsi
yo
x+2y+zh
2z
Wherein 1.10≤y:x≤1.50,0.97≤x:z≤1.50.The sample obtained is the particle of 100nm ~ 2 μm, and specific area is 140 ~ 200m
2/ g.It is adsorbed on about 10 minutes close to balance, clearance ﹥ 90% when 120 minutes to methylene blue, and maximal absorptive capacity is 280 ~ 365mg/g, far above the maximum adsorption value of about 100mg/g of other magnesium silicate products not using template equally.
The preparation method of nanometer magnesium silicate sorbing material provided by the invention, concrete steps are as follows:
A. with the sodium silicate solution of deionized water preparation 0.1 ~ 0.4mol/L, more isopyknic 0.1 ~-0.4mol/L magnesium salt solution solution is prepared; Described magnesium salts is MgCl
2, Mg (NO
3)
2or MgSO
4in one.
B. being added in liquid film reactor by the flow velocity of 1000mL/min by two solution in steps A makes it mix, the spinner velocity 1000 ~ 5000r/min of liquid film reactor, rotor and stator spacing 0.1 ~ 0.5mm, fast nucleation 1 ~ 3min;
C. the mixed serum that step B obtains is proceeded to the hydrothermal reaction kettle that band stirs, be heated to 150 ~ 190 DEG C, under low whipping speed 0 ~ 300r/min, hydro-thermal reaction 8 ~ 16h;
D. slurries are naturally cooled to room temperature after terminating by reaction, centrifugal, with 100mL deionized water washing 3 ~ 5 times, the product after washing is placed in 40 ~ 120 DEG C of dry 24h of baking oven, namely obtains nanometer magnesium silicate efficient adsorption material.
Characterize the product obtained with X-ray diffraction (XRD), obtain Fig. 1, result shows the method and successfully synthesizes magnesium silicate material; As can be seen from scanning electron microscope image (SEM) Fig. 2 a, the product obtained is the rice granular solid matter of about 200nm.
The absorption property test of nanometer magnesium silicate: add the methylene blue solution 50mL that concentration is 100 ~ 300mg/L in conical flask, by conical flask as on shaking table, constant temperature water bath 25 DEG C, jolts speed 160r/min.Add nanometer magnesium silicate 33mg prepared by step D, adsorption reaction starts.Respectively negate should start after 2,5,10,20,45,90, the solution of 120min, with centrifuge centrifugal 2min under 1500r/min condition, obtain supernatant.Detect not supernatant in the same time with UV-Vis (ultraviolet-visible absorption spectroscopy) and, in the absorbance at wavelength 664nm (characteristic absorption wavelength of methylene blue) place, obtain not the methylene blue concentration (C in solution in the same time with this
t) and magnesium silicate product to the adsorbance (Q of methylene blue
e), wherein:
C
0for adsorbing the initial concentration (100 ~ 300mg/L) of front methylene blue solution, C
tfor the concentration of not Methylene Blue in Solution in the same time, V is the volume (50mL) of methylene blue solution, and m is the quality (33mg) of added magnesium silicate sample.Measurement result is shown in Fig. 3, table 1.Fig. 3 is the measurement result of embodiment 1, and table 1 is the adsorption test related data of embodiment 1 ~ 5.Shown by Fig. 3 and table 1, the adsorption of magnesium silicate material that the present invention obtains rapidly and efficiently can complete the absorption to methylene blue, and adsorption reaction is at 10 minutes namely close to balance, and clearance ﹥ 90% when 120 minutes, maximal absorptive capacity is 280 ~ 365mg/g.
The invention has the beneficial effects as follows: in the preparation process of magnesium silicate, introduce rotating liquid-film reactor first, then by the improvement to preparation condition, regulation and control, finally obtained the nanometer magnesium silicate sorbing material of grain of rice shape.Its nanometer silicic acid magnesium products obtained compared to the template adopted has better adsorption capacity, and overcomes the shortcoming being not easy to large-scale production, has the potentiality of wide practical application.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of magnesium silicate prepared by embodiment 1.
The SEM of Fig. 2 magnesium silicate contrasts photo, a is embodiment 1, and b is comparative example.
Fig. 3 is that embodiment 1 gained magnesium silicate is to methylene blue solution (C
0=200mg/L) absorption property curve map.
Detailed description of the invention
Embodiment 1
Steps A: take 10.256g (40mmol) Mg (NO
3)
26H
2o and 11.369g (40mmol) Na
2siO
39H
2o is dissolved in 200mL deionized water respectively, fully stirs, and makes it dissolve.
Step B: pour two solution of steps A into liquid film reactor with the flow velocity equal-volume of 1000mL/min, turns rotor speed 4000rpm, rotor-stator spacing 0.1mm, rapid mixing 2min.
Step C: above-mentioned slurries are transferred to the hydrothermal reaction kettle that band stirs, programming rate 1 DEG C/min, is slowly warming up to 170 DEG C, constant temperature 12h, mixing speed 100r/min.
Step D: the slurries after having reacted are naturally cooled to room temperature, centrifugal, spend after 100mL deionized water washs 3 times, then in 60 DEG C of baking ovens dry 24h, namely obtain nanometer magnesium silicate sorbing material.
Fig. 1 is the nanometer magnesium silicate XRD analysis result of preparation, and the magnesium silicate shown in its with standard card JCPDS no.03-0174 is corresponding, and its chemical formula is Mg
3si
4o
13h
4.The SEM image of Fig. 2 a shows, obtained magnesium silicate is the rice granular solid matter of about 200nm. adopting low temperature nitrogen absorption method (BET) to test its specific area is 197.63m
2/ g.It sees Fig. 3 and table 1 to the Absorbency Test data of methylene blue solution.In order to test the maximal absorptive capacity of product, added an examination of initial concentration C
0=228mg/L and C
0two groups of adsorption experiments during=276mg/L, data are in table 1.
Embodiment 2
Steps A: take 8.132g (40mmol) MgCl
26H
2o and 11.369g (40mmol) Na
2siO
39H
2o is dissolved in 200mL deionized water respectively, fully stirs, and makes it dissolve.
Step B: pour two solution of steps A into liquid film reactor by the flow velocity equal-volume of 1000mL/min, turns rotor speed 4000r/min, rotor-stator spacing 0.1mm, fast nucleation 2min.
Step C: above-mentioned slurries are transferred to the hydrothermal reaction kettle that band stirs, programming rate about 1 DEG C/min, is slowly warming up to 170 DEG C, under low whipping speed 100r/min, constant temperature 12h.
Step D: the slurries after having reacted are naturally cooled to room temperature, centrifugal, spend after 100mL deionized water washs 5 times, with liquor argenti nitratis ophthalmicus chlorine detection ion without visible precipitate, then in 60 DEG C of baking ovens dry 24h, namely obtain nanometer magnesium silicate sorbing material.
XRD analysis shows, obtained product corresponds to the magnesium silicate shown in standard card JCPDS no.03-0174, and its chemical formula is Mg
3si
4o
13h
4.SEM image shows, and obtained magnesium silicate is the rice granular solid matter of about 200nm; It is 190.23m that BET records specific area
2/ g.Its to the Absorbency Test data of methylene blue solution in table 1.
Embodiment 3
Steps A: take 4.815g MgSO
4(40mmol) with 11.369g Na
2siO
39H
2o (40mmol) is dissolved in 200mL deionized water respectively, fully stirs, and makes it dissolve.
Step B: pour two solution of steps A into liquid film reactor by the flow velocity equal-volume of 1000mL/min, turns rotor speed 4000r/min, rotor-stator spacing 0.1mm, fast nucleation 2min.
Step C: above-mentioned slurries are transferred to the hydrothermal reaction kettle that band stirs, programming rate 1 DEG C/min, is slowly warming up to 170 DEG C, constant temperature 12h, mixing speed 100r/min.
Step D: the slurries after having reacted are naturally cooled to room temperature, centrifugal, spend after 100mL deionized water washs 5 times, detect sulfate ion without visible precipitate with barium nitrate solution, then in 60 DEG C of baking ovens dry 24h, namely obtain nanometer magnesium silicate sorbing material.
XRD analysis shows, obtained product corresponds to the magnesium silicate shown in standard card JCPDS no.03-0174, and its chemical formula is Mg
3si
4o
13h
4.SEM image shows, and obtained magnesium silicate is the rice granular solid matter of about 200nm; It is 187.73m that BET records specific area
2/ g.Its to the Absorbency Test data of methylene blue solution in table 1.
Embodiment 4
Steps A: take 4.066g (20mmol) MgCl
26H
2o and 8.526g (30mmol) Na
2siO
39H
2o is dissolved in 200mL deionized water respectively, fully stirs, and makes it dissolve.
Step B: pour two solution of steps A into liquid film reactor with the flow velocity equal-volume of 1000mL/min, turns rotor speed 3000rpm, rotor-stator spacing 0.2mm, rapid mixing 1min.
Step C: above-mentioned slurries are transferred to the hydrothermal reaction kettle that band stirs, programming rate 1 DEG C/min, is slowly warming up to 190 DEG C, constant temperature 12h, mixing speed 300r/min.
Step D: the slurries after having reacted are naturally cooled to room temperature, centrifugal, spend after 100mL deionized water washs 3 times, then in 80 DEG C of baking ovens dry 24h, namely obtain nanometer magnesium silicate sorbing material.
XRD analysis shows, obtained sample corresponds to the magnesium silicate shown in standard card JCPDS no.02-0048, and chemical formula is Mg
2si
3o
10h
4.SEM image shows, obtained magnesium silicate is the shuttle shape particle of about 200nm; It is 162.79m that BET records specific area
2/ g.Its to the Absorbency Test data of methylene blue solution in table 1.
Comparative example
In order to contrast nucleation-crystallization isolation method to the impact of product morphology, changed into by the step B of embodiment 1 and with normal agitation, two solution are mixed, mixing speed 1000r/min, other steps are all identical with embodiment 1.
XRD analysis shows, obtained sample corresponds to the magnesium silicate shown in standard card JCPDS no.03-0174, and chemical formula is Mg
3si
4o
13h
4; Its SEM image is shown in Fig. 2 b, finds out that this magnesium silicate is irregular block structure by figure; It is 46.8m that BET records specific area
2/ g.Its to the Absorbency Test data of methylene blue solution in table 1.
Table 1
Claims (3)
1. a preparation method for nanometer magnesium silicate sorbing material, concrete steps are as follows:
A. with the sodium silicate solution of deionized water preparation 0.1 ~ 0.4mol/L, more isopyknic 0.1 ~ 0.4mol/L magnesium salt solution solution is prepared; Described magnesium salts is MgCl
2, Mg (NO
3)
2or MgSO
4in one;
B. being added in liquid film reactor by the flow velocity of 1000mL/min by two solution in steps A makes it mix, the spinner velocity 1000 ~ 5000r/min of liquid film reactor, rotor and stator spacing 0.1 ~ 0.5mm, fast nucleation 1 ~ 3min;
C. the mixed serum that step B obtains is proceeded to the hydrothermal reaction kettle that band stirs, be heated to 150 ~ 190 DEG C, under low whipping speed 0 ~ 300r/min, hydro-thermal reaction 8 ~ 16h;
D. slurries are naturally cooled to room temperature after terminating by reaction, centrifugal, with 100mL deionized water washing 3 ~ 5 times, the product after washing is placed in 40 ~ 120 DEG C of dry 24h of baking oven, namely obtains nanometer magnesium silicate sorbing material.
2. the nanometer magnesium silicate sorbing material prepared of method according to claim 1, its chemical general formula is: Mg
xsi
yo
x+2y+zh
2z, wherein 1.10≤y:x≤1.50,0.97≤x:z≤1.50; This material is the particle of 100nm ~ 2 μm, and specific area is 140 ~ 200m
2/ g.
3. the nanometer magnesium silicate sorbing material prepared of a method according to claim 1, it is characterized in that this material balances the adsorption reaction of water Methylene Blue is close at about 10 minutes, clearance ﹥ 90% when 120 minutes, maximal absorptive capacity is 280 ~ 365mg/g.
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Cited By (8)
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| CN107381869A (en) * | 2017-08-21 | 2017-11-24 | 北京市畜牧业环境监测站 | A kind of method for handling methylene blue waste water |
| CN108067182A (en) * | 2017-11-13 | 2018-05-25 | 南京凯特莱斯环保科技有限公司 | A kind of porous silicic acid magnesium composite adsorption film and preparation method thereof |
| CN109880632A (en) * | 2019-03-08 | 2019-06-14 | 北京世纪阿姆斯生物工程有限公司 | It is acidified hardened soil remediation microbial inoculum and preparation method thereof and application method |
| CN110170298A (en) * | 2019-05-29 | 2019-08-27 | 北京化工大学常州先进材料研究院 | A kind of method that slurry composite algorithm prepares magnesium silicate magnesium carbonate composite adsorbing material |
| CN110180495A (en) * | 2019-05-29 | 2019-08-30 | 北京化工大学常州先进材料研究院 | A kind of method that polynary coprecipitation prepares magnesium silicate based composite adsorption material |
| CN113198415A (en) * | 2020-02-27 | 2021-08-03 | 合肥三利谱光电科技有限公司 | Preparation method of adsorption material for sewage treatment |
| CN115124047A (en) * | 2022-04-22 | 2022-09-30 | 上海市农业科学院 | Magnesium silicate gel and preparation method and application thereof |
| CN115364826A (en) * | 2021-05-21 | 2022-11-22 | 安庆北化大科技园有限公司 | Preparation method of super-hydrophobic porous magnesium silicate oil-water separation material, prepared material and application thereof |
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Cited By (13)
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| CN107381869A (en) * | 2017-08-21 | 2017-11-24 | 北京市畜牧业环境监测站 | A kind of method for handling methylene blue waste water |
| CN108067182A (en) * | 2017-11-13 | 2018-05-25 | 南京凯特莱斯环保科技有限公司 | A kind of porous silicic acid magnesium composite adsorption film and preparation method thereof |
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| CN109880632A (en) * | 2019-03-08 | 2019-06-14 | 北京世纪阿姆斯生物工程有限公司 | It is acidified hardened soil remediation microbial inoculum and preparation method thereof and application method |
| CN110180495B (en) * | 2019-05-29 | 2022-04-12 | 北京化工大学常州先进材料研究院 | Method for preparing magnesium silicate based composite adsorption material by multi-coprecipitation method |
| CN110170298A (en) * | 2019-05-29 | 2019-08-27 | 北京化工大学常州先进材料研究院 | A kind of method that slurry composite algorithm prepares magnesium silicate magnesium carbonate composite adsorbing material |
| CN110180495A (en) * | 2019-05-29 | 2019-08-30 | 北京化工大学常州先进材料研究院 | A kind of method that polynary coprecipitation prepares magnesium silicate based composite adsorption material |
| CN110170298B (en) * | 2019-05-29 | 2022-03-18 | 北京化工大学常州先进材料研究院 | Method for preparing magnesium silicate magnesium carbonate composite adsorption material by slurry state composite method |
| CN113198415A (en) * | 2020-02-27 | 2021-08-03 | 合肥三利谱光电科技有限公司 | Preparation method of adsorption material for sewage treatment |
| CN115364826A (en) * | 2021-05-21 | 2022-11-22 | 安庆北化大科技园有限公司 | Preparation method of super-hydrophobic porous magnesium silicate oil-water separation material, prepared material and application thereof |
| CN115364826B (en) * | 2021-05-21 | 2023-10-03 | 安庆北化大科技园有限公司 | Preparation method of super-hydrophobic porous magnesium silicate oil-water separation material, prepared material and application thereof |
| CN115124047A (en) * | 2022-04-22 | 2022-09-30 | 上海市农业科学院 | Magnesium silicate gel and preparation method and application thereof |
| CN115124047B (en) * | 2022-04-22 | 2023-11-03 | 上海市农业科学院 | Magnesium silicate gel and preparation method and application thereof |
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