CN103933938A - Preparation method of magnesium silicate/carbon composite material - Google Patents
Preparation method of magnesium silicate/carbon composite material Download PDFInfo
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- CN103933938A CN103933938A CN201410155074.2A CN201410155074A CN103933938A CN 103933938 A CN103933938 A CN 103933938A CN 201410155074 A CN201410155074 A CN 201410155074A CN 103933938 A CN103933938 A CN 103933938A
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- magnesium silicate
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Abstract
The invention relates to a preparation method of a magnesium silicate/carbon composite material. The preparation method comprises the following steps: dropwise adding a soluble magnesium salt solution into a sodium silicate solution, and evenly stirring to obtain magnesium silicate gel; under the condition of stirring, dropwise adding a carbon source solution into the magnesium silicate gel to obtain a magnesium silicate/carbon mixed solution; carrying out closed reaction on the magnesium silicate/carbon mixed solution at 150-250 DEG C for 40-72h to obtain magnesium silicate/carbon composite gel; carrying out suction filtration, centrifugal separation or filter pressing treatment on the magnesium silicate/carbon composite gel, washing, drying and grinding to obtain the magnesium silicate/carbon composite material. According to the preparation method provided by the invention, modification treatment is carried out on pure magnesium silicate, the preparation of a novel magnesium silicate inorganic composite material is realized, and the prepared magnesium silicate/carbon composite material has a large pore diameter and strong adsorption capability for macromolecular organic pigment; the preparation method is easy to operate, mild in conditions, safe and reliable, higher in yield, and suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium silicate/carbon composite, belong to inorganic chemistry mesosilicic acid salt composite preparing technical field.
Background technology
Recent year chemical industry, medicine, food service industry get more and more to the demand of adsorbent, in the face of the demand in market and application widely, sorbent material are had higher requirement.In conventional decolorizing adsorbent, the effect of active carbon is better, but simple acticarbon price is more expensive, and magnesium silicate gel is wide as a kind of inorganic material source, low price.Magnesium silicate/carbon composite molecular formula is 2MgO.nSiO
2.xH
2o/C, is a kind of unformed composite particles of loose structure, has larger aperture.Can adsorb large molecule organic pigment, good to the pigment stink adsorption effect in organic solvent, can be applied in addition food grease field.Chinese patent literature CN101613110A discloses a kind of aluminum-magnesium silicate compound and synthetic method thereof; the magnesium of its aluminium that contains 14.28%-18.79% weight content, 6.86%-16.71% weight content, the silicon of 6.73%-16.64% weight content; and magnalium ratio is 0.5-1.2 or 1.4-2.8; the method comprises that (1) is by water-soluble respectively to magnesium sulfate and aluminum sulfate, and gained solution mixes and stirs; (2) by water-soluble sodium metasilicate one-tenth sodium silicate solution, add sodium hydroxide solution, after stirring, be added in step (1) and react; (3) calcium chloride solid or the aqueous solution are added to stirring reaction in step (2) reaction mass, form described aluminium-magnesium silicate.This invention overcomes the deficiency of extracting aluminium-magnesium silicate from natural ore deposit, can obtain the product of high-purity medical level.
At present, be not reported about the preparation of magnesium silicate/carbon composite.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of preparation method of magnesium silicate/carbon composite.
Technical scheme of the present invention is as follows:
A preparation method for magnesium silicate/carbon composite, comprises that step is as follows:
(1) be 1:(1.5-3.5 by the mol ratio of magnesia and silica), soluble magnesium salting liquid is splashed in sodium silicate solution, stir, make magnesium silicate gel;
(2), under stirring condition, be 1:(1～15 by the mol ratio of magnesium silicate and carbon atom), carbon source solution is splashed in the magnesium silicate gel that step (1) makes, make magnesium silicate/carbon mixed solution; Described carbon source is glucose or sucrose;
(3) magnesium silicate/carbon mixed solution step (2) being made is in 150-250 DEG C, and confined reaction 40-72h, makes magnesium silicate/carbon plural gel;
(4) magnesium silicate/carbon plural gel suction filtration, centrifugation or the press filtration that step (3) are made, washing, dry, grind, obtain magnesium silicate/carbon composite.
According to the present invention, preferred, the solubility magnesium salts described in step (1) is magnesium sulfate, magnesium nitrate or magnesium chloride, and the concentration of described soluble magnesium salting liquid is 0.25～0.45mol/L;
The concentration of described sodium silicate solution is 0.45～0.7mol/L, and the modulus of described sodium silicate solution is 1.0～3.5;
The drop rate of described soluble magnesium salting liquid is 4～6ml/min.
According to the present invention, preferred, the mol ratio of the magnesium silicate described in step (2) and carbon atom is 1:(1.5～5).
The concentration of described carbon source solution is 7～15wt%, more preferably 10wt%; The drop rate of described carbon source solution is 10～15ml/min.
According to the present invention, preferred, the reaction temperature described in step (3) is 180-220 DEG C, further preferably 200 DEG C; Reaction time is 48-60h; Preferably, reaction pH is 8～13.
According to the present invention, preferred, washing to washings pH6.5-7.5 described in step (4); Baking temperature is 90-150 DEG C, drying time 12-36h.Being ground to particle diameter is 20-250 μ m.
Beneficial effect of the present invention:
1, the present invention carries out modification to simple magnesium silicate, has realized a kind of preparation of novel magnesium silicate composite inorganic material, and the magnesium silicate/carbon composite aperture making is large, to the high adsorption capacity of large molecule organic pigment.
2, simple to operate, the mild condition, safe and reliable of the inventive method, and productive rate is higher, is applicable to industrialized production.
3, raw material of the present invention is cheap and easy to get, low production cost.
Brief description of the drawings
Fig. 1 is the pore size distribution curve of magnesium silicate/carbon composite of preparing of the embodiment of the present invention 1.
Fig. 2 is the pore size distribution curve of the magnesium silicate material prepared of comparative example of the present invention.
Fig. 3 is the adsorption curve figure of comparative example and embodiment 1 in experimental example 1 of the present invention, the adsorption curve that wherein a is comparative example, and b is the adsorption curve of embodiment 1.
Detailed description of the invention
Below by specific embodiment, the present invention will be further described, but be not limited to this.
Raw materials usedly in embodiment be conventional raw material, device therefor is conventional equipment, commercial product.
Embodiment 1
A preparation method for magnesium silicate/carbon composite, comprises that step is as follows:
(1) by 8.9735g Mg (NO
3)
2.6H
2o dissolved dilution is made into the solution of concentration (taking magnesia) as 0.35mol/L in 100ml water, by 12.8421g Na
2siO
3.9H
2o dissolved dilution is made into the solution of concentration (taking silica) as 0.45mol/L in 100ml water, by 5g C
6h
12o
6.H
2the mass fraction that O is made into is 10% solution;
In three mouthfuls of reaction bulbs of 250ml by 40ml Mg (NO
3)
2.6H
2o solution is added drop-wise to the Na of 56ml with the speed of 5ml/min
2siO
3.9H
2in O solution, stir, make magnesium silicate gel;
(2) under stirring condition, in the magnesium silicate gel making to step (1), drip the glucose solution 150ml of 10wt% concentration with the speed of 10ml/min, drip rear continuation and stir 15min, make magnesium silicate/carbon mixed solution;
(3) magnesium silicate/carbon mixed solution step (2) being made evenly joins in 2 100ml hydrothermal reaction kettles, and being put into and regulating reaction temperature in baking oven is 200 DEG C, and confined reaction 48h, makes magnesium silicate/carbon plural gel;
(4) magnesium silicate/carbon plural gel suction filtration step (3) being made, washing is extremely neutral, 120 DEG C of dry 14h, being ground to particle diameter is 100～200 μ m, obtains magnesium silicate/carbon composite.
Magnesium silicate/carbon composite test pore size distribution curve prepared by the present embodiment, as shown in Figure 1.As shown in Figure 1, magnesium silicate/carbon composite aperture that prepared by the present embodiment is larger.
Embodiment 2
A preparation method for magnesium silicate/carbon composite, comprises that step is as follows:
(1) by 4.2234g MgSO
4dissolved dilution is made into the solution of concentration (taking magnesia) as 0.35mol/L in 100ml water, by 18.4733g Na
2siO
3.9H
2o dissolved dilution is made into the solution of concentration (taking silica) as 0.65mol/L in 100ml water, by 15g C
6h
12o
6.H
2it is 10% solution 150ml that O is made into mass fraction;
In three mouthfuls of reaction bulbs of 500ml by the MgSO of 80ml
4solution is added drop-wise to the Na of 86.2ml with the speed of 4ml/min
2siO
3.9H
2in O solution, stir, make magnesium silicate gel;
(2) under stirring condition, in the magnesium silicate gel making to step (1), drip the glucose solution 100ml of 10wt% concentration with the speed of 15ml/min, drip rear continuation and stir 20min, make magnesium silicate/carbon mixed solution;
(3) magnesium silicate/carbon mixed solution step (2) being made evenly joins in 2 100ml hydrothermal reaction kettles, and being put into and regulating reaction temperature in baking oven is 200 DEG C, and confined reaction 50h, makes magnesium silicate/carbon plural gel;
(4) magnesium silicate/carbon plural gel suction filtration step (3) being made, washing is extremely neutral, 120 DEG C of dry 24h, being ground to particle diameter is 100～180 μ m, obtains magnesium silicate/carbon composite.
Embodiment 3
A preparation method for magnesium silicate/carbon composite, comprises that step is as follows:
(1) by 8.9735g Mg (NO
3)
2.6H
2o dissolved dilution is made into the solution of concentration (taking magnesia) as 0.35mol/L in 100ml water, by 12.8421g Na
2siO
3.9H
2o dissolved dilution is made into the solution of concentration (taking silica) as 0.45mol/L in 100ml water, by 5g C
6h
12o
6.H
2the mass fraction that O is made into is 10% solution;
In three mouthfuls of reaction bulbs of 250ml by 40ml Mg (NO
3)
2.6H
2o solution is added drop-wise to the Na of 108ml with the speed of 5ml/min
2siO
3.9H
2in O solution, stir, make magnesium silicate gel;
(2) under stirring condition, in the magnesium silicate gel making to step (1), drip the glucose solution 50ml of 10wt% concentration with the speed of 12ml/min, drip rear continuation and stir 15min, make magnesium silicate/carbon mixed solution;
(3) magnesium silicate/carbon mixed solution step (2) being made evenly joins in 2 100ml hydrothermal reaction kettles, and being put into and regulating reaction temperature in baking oven is 250 DEG C, and confined reaction 40h, makes magnesium silicate/carbon plural gel;
(4) magnesium silicate/carbon plural gel suction filtration step (3) being made, washing is extremely neutral, 110 DEG C of dry 24h, being ground to particle diameter is 80～150 μ m, obtains magnesium silicate/carbon composite.
Embodiment 4
A preparation method for magnesium silicate/carbon composite, comprises that step is as follows:
(1) by 4.2234g MgSO
4dissolved dilution is made into the solution of concentration (taking magnesia) as 0.35mol/L in 100ml water, by 18.4733g Na
2siO
3.9H
2o dissolved dilution is made into the solution of concentration (taking silica) as 0.65mol/L in 100ml water, by 15g C
6h
12o
6.H
2it is 10% solution 150ml that O is made into mass fraction;
In three mouthfuls of reaction bulbs of 500ml by the MgSO of 80ml
4solution is added drop-wise to the Na of 64ml with the speed of 4ml/min
2siO
3.9H
2in O solution, stir, make magnesium silicate gel;
(2) under stirring condition, in the magnesium silicate gel making to step (1), drip the glucose solution 100ml of 10wt% concentration with the speed of 10ml/min, drip rear continuation and stir 20min, make magnesium silicate/carbon mixed solution;
(3) magnesium silicate/carbon mixed solution step (2) being made evenly joins in 2 100ml hydrothermal reaction kettles, and being put into and regulating reaction temperature in baking oven is 180 DEG C, and confined reaction 60h, makes magnesium silicate/carbon plural gel;
(4) magnesium silicate/carbon plural gel suction filtration step (3) being made, washing is extremely neutral, 110 DEG C of dry 24h, being ground to particle diameter is 80～150 μ m, obtains magnesium silicate/carbon composite.
Comparative example
Do not add carbon source and carry out modification, prepare magnesium silicate material, step is as follows:
(1) by 8.9735g Mg (NO
3)
2.6H
2o dissolved dilution is made into the solution of concentration (taking magnesia) as 0.35mol/L in 100ml water, by 12.8421g Na
2siO
3.9H
2o dissolved dilution is made into the solution of concentration (taking silica) as 0.45mol/L in 100ml water;
In three mouthfuls of reaction bulbs of 250ml by 40ml Mg (NO
3)
2.6H
2o solution is added drop-wise to the Na of 56ml with the speed of 5ml/min
2siO
3.9H
2in O solution, stir, make magnesium silicate gel;
(2) magnesium silicate gel step (1) being made evenly joins in 2 100ml hydrothermal reaction kettles, and being put into and regulating reaction temperature in baking oven is 200 DEG C, and confined reaction 48h, makes magnesium silicate gel;
(3) magnesium silicate gel suction filtration step (2) being made, washing is extremely neutral, 100 DEG C of dry 24h, being ground to particle diameter is 100～120um, obtains magnesium silicate gel rubber material.
Magnesium silicate testing of materials pore size distribution curve prepared by this comparative example, as shown in Figure 2.As shown in Figure 2, the magnesium silicate material aperture that prepared by this comparative example is less.
The pore size distribution data of embodiment 1 and comparative example is as shown in table 1.
Table 1
| Sample title | Specific area m 2/g | Average pore size nm |
| Comparative example | 328.1116 | 18.2865 |
| Embodiment 1 | 170.3182 | 35.2282 |
Experimental example 1
Magnesium silicate material prepared by magnesium silicate/carbon composite prepared by embodiment 1 and comparative example carries out absorption property test,
Taking n-hexane as solvent configures certain density organic pigment solution, add respectively magnesium silicate and the magnesium silicate/carbon adsorbent of equivalent, the adsorption curve once obtaining under identical adsorption time.Adsorption curve as shown in Figure 3, the adsorption curve that wherein a is comparative example, b is the adsorption curve of embodiment 1, the result of equilibrium adsorption capacity is as shown in table 2.From Fig. 3 and table 2, the magnesium silicate material that the equilibrium adsorption capacity of magnesium silicate/carbon composite prepared by embodiment 1 is prepared than comparative example is obviously larger.
Table 2
| Project/numbering | Comparative example | Embodiment 1 |
| Adsorbance (mg/g) | 97.6 | 312 |
Claims (8)
1. a preparation method for magnesium silicate/carbon composite, comprises that step is as follows:
(1) be 1:(1.5-3.5 by the mol ratio of magnesia and silica), soluble magnesium salting liquid is splashed in sodium silicate solution, stir, make magnesium silicate gel;
(2), under stirring condition, be 1:(1～15 by the mol ratio of magnesium silicate and carbon atom), carbon source solution is splashed in the magnesium silicate gel that step (1) makes, make magnesium silicate/carbon mixed solution; Described carbon source is glucose or sucrose;
(3) magnesium silicate/carbon mixed solution step (2) being made is in 150-250 DEG C, and confined reaction 40-72h, makes magnesium silicate/carbon plural gel;
(4) magnesium silicate/carbon plural gel suction filtration, centrifugation or the press filtration that step (3) are made, washing, dry, grind, obtain magnesium silicate/carbon composite.
2. the preparation method of magnesium silicate/carbon composite according to claim 1, is characterized in that, the solubility magnesium salts described in step (1) is magnesium sulfate, magnesium nitrate or magnesium chloride, and the concentration of described soluble magnesium salting liquid is 0.25～0.45mol/L.
3. the preparation method of magnesium silicate/carbon composite according to claim 1, is characterized in that, the concentration of the sodium silicate solution described in step (1) is 0.45～0.7mol/L, and the modulus of described sodium silicate solution is 1.0～3.5.
4. the preparation method of magnesium silicate/carbon composite according to claim 1, is characterized in that, the drop rate of the soluble magnesium salting liquid described in step (1) is 4～6ml/min.
5. the preparation method of magnesium silicate/carbon composite according to claim 1, is characterized in that, the mol ratio of the magnesium silicate described in step (2) and carbon atom is 1:(1.5～5).
6. the preparation method of magnesium silicate/carbon composite according to claim 1, is characterized in that, the concentration of the carbon source solution described in step (2) is 7～15wt%, and the drop rate of described carbon source solution is 10～15ml/min.
7. the preparation method of magnesium silicate/carbon composite according to claim 1, is characterized in that, the reaction temperature described in step (3) is 180-220 DEG C; Reaction time is 48-60h.
8. the preparation method of magnesium silicate/carbon composite according to claim 1, is characterized in that, washing to washings pH6.5-7.5 described in step (4); Baking temperature is 90-150 DEG C, drying time 12-36h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| EP3341107B1 (en) | 2015-08-28 | 2020-12-30 | Imerys Filtration Minerals, Inc. | High permeability composite magnesium silicate filter aids |
| CN113578266A (en) * | 2021-08-05 | 2021-11-02 | 福州大学 | Preparation and application of nano magnesium silicate biochar |
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| CN102442878A (en) * | 2010-10-12 | 2012-05-09 | 中国石油化工股份有限公司 | Purification method of dichloromethane |
| CN102688780A (en) * | 2012-06-04 | 2012-09-26 | 昆明理工大学 | Method for preparing organic and inorganic composite mesoporous solid base catalyst |
| JP2013166133A (en) * | 2012-02-16 | 2013-08-29 | Kotegawa Sangyo Kk | Acidic gas remover and method of removing acidic gas |
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2014
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102442878A (en) * | 2010-10-12 | 2012-05-09 | 中国石油化工股份有限公司 | Purification method of dichloromethane |
| JP2013166133A (en) * | 2012-02-16 | 2013-08-29 | Kotegawa Sangyo Kk | Acidic gas remover and method of removing acidic gas |
| CN102688780A (en) * | 2012-06-04 | 2012-09-26 | 昆明理工大学 | Method for preparing organic and inorganic composite mesoporous solid base catalyst |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3341107B1 (en) | 2015-08-28 | 2020-12-30 | Imerys Filtration Minerals, Inc. | High permeability composite magnesium silicate filter aids |
| EP3341107B2 (en) † | 2015-08-28 | 2023-10-18 | Imerys Filtration Minerals, Inc. | High permeability composite magnesium silicate filter aids |
| 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 |
| CN108067182B (en) * | 2017-11-13 | 2020-06-09 | 南京凯特莱斯环保科技有限公司 | Porous magnesium silicate composite adsorption film and preparation method thereof |
| 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 |
| 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 |
| CN113578266A (en) * | 2021-08-05 | 2021-11-02 | 福州大学 | Preparation and application of nano magnesium silicate biochar |
| CN113578266B (en) * | 2021-08-05 | 2023-02-28 | 福州大学 | Preparation and application of nano magnesium silicate biochar |
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