CN113120914A - Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate - Google Patents

Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate Download PDF

Info

Publication number
CN113120914A
CN113120914A CN202010041192.6A CN202010041192A CN113120914A CN 113120914 A CN113120914 A CN 113120914A CN 202010041192 A CN202010041192 A CN 202010041192A CN 113120914 A CN113120914 A CN 113120914A
Authority
CN
China
Prior art keywords
magnesium silicate
ball milling
agate
equal
porous
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.)
Withdrawn
Application number
CN202010041192.6A
Other languages
Chinese (zh)
Inventor
冯拥军
李彧奇
李殿卿
汪杰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anqing Beihuada Science And Technology Park Co ltd
Beijing University of Chemical Technology
Original Assignee
Anqing Beihuada Science And Technology Park Co ltd
Beijing University of Chemical Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Anqing Beihuada Science And Technology Park Co ltd, Beijing University of Chemical Technology filed Critical Anqing Beihuada Science And Technology Park Co ltd
Priority to CN202010041192.6A priority Critical patent/CN113120914A/en
Publication of CN113120914A publication Critical patent/CN113120914A/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/22—Magnesium silicates
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • 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
    • C02F2101/20—Heavy metals or heavy metal compounds
    • 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
    • C02F2101/30—Organic compounds
    • C02F2101/308—Dyes; Colorants; Fluorescent agents
    • 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
    • C02F2101/30—Organic compounds
    • C02F2101/38—Organic compounds containing nitrogen

Abstract

The invention discloses a method for preparing porous magnesium silicate by using a ball milling method, which relates to the technical field of preparation of inorganic functional materials. The invention also provides magnesium silicate prepared by the preparation method. The invention has the beneficial effects that: the magnesium silicate obtained by the invention is in a sheet shape with the thickness of about 200nm, and the specific surface area reaches 800m2·g‑1The porous material has the excellent characteristics of large pore structure, large specific surface area, charge on the surface and the like. Wherein for Cu2+The adsorption rate of the adsorbent can reach more than 80 percent, and the maximum adsorption capacity can reach 223.05 mg/g. For methylene blueThe maximum adsorption capacity can reach 300 mg/g. The preparation process does not need any solvent or heating treatment, is energy-saving and environment-friendly, is easy for large-scale application and large-scale industrial production, and has wide application prospect in the aspect of sewage treatment.

Description

Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate
Technical Field
The invention relates to the technical field of preparation of inorganic functional materials, in particular to a method for preparing porous magnesium silicate by using a ball milling method and prepared magnesium silicate.
Background
Water pollution is one of the problems in the current social development which needs to be solved urgently, and harmful organic dyes and toxic heavy metal ions discharged by industry are the most important parts for treating water pollution at present, and directly threaten the production life and the body health of human beings. The development of efficient and feasible sewage treatment technology is a major problem to be solved urgently in the current society.
The most important current methods for sewage treatment are physical adsorption, biodegradation and chemical methods. Of these, the physical adsorption method is one of the most economical and practical methods. The key point of the method is to develop an efficient and cheap adsorbing material which is green and environment-friendly and can be repeatedly utilized to a certain extent. Among the current adsorption materials, magnesium silicate has a special microstructure, and has charges on the surface thereof, so that the magnesium silicate can strongly adsorb positive ions, and the magnesium silicate attracts people's attention for a while.
The adsorption performance of magnesium silicate is mainly related to its morphology, pore structure and the charge amount carried on its surface, and different synthesis methods can cause significant changes in these parameters of magnesium silicate.
Literature (Huang, R, ACS Sustainable chem. Eng.2017,5,2774-2780.) preparation of layered nano-materials of magnesium silicate with high specific surface area and large pore diameter in mixed solvent of ethanol and water for Cu2+The maximum adsorption capacity of (2) was 52.3 mg/g. The literature (Wenbo Wang, Chemical Engineering Journal) designs a novel adsorbent, and the natural spore powder is modified by adopting a one-step hydrothermal method, and for Cu2+The maximum adsorption capacity at 50ppm is only 50 mg/g. Literature (Renyao Huang, ACS App)l. mater. interfaces 2018,10,22776-2+The maximum adsorption rate of the adsorbent is only about 110 mg/g.
Patent CN201410155074.2 discloses a method for preparing magnesium silicate/carbon composite material, which comprises dripping soluble magnesium salt solution into sodium silicate solution, stirring well to obtain magnesium silicate gel; under the condition of stirring, dripping a carbon source solution into the magnesium silicate gel to prepare a magnesium silicate/carbon mixed solution; performing closed reaction on the magnesium silicate/carbon mixed solution at the temperature of 150 ℃ and 250 ℃ for 40-72h to prepare magnesium silicate/carbon composite gel; the magnesium silicate/carbon composite gel is subjected to suction filtration, centrifugal separation or filter pressing treatment, washing, drying and grinding to obtain the magnesium silicate/carbon composite gel.
Disclosure of Invention
One of the technical problems to be solved by the invention is that the existing magnesium silicate preparation method needs to dissolve and heat up raw materials, and provides a preparation method of magnesium silicate without dissolution and heating.
The invention solves the technical problems through the following technical means:
a method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) mixing a solid compound containing magnesium element with a sodium silicate solid, and pouring the mixture into an agate ball milling tank;
(2) placing agate balls into the agate ball milling tank in the step (1) and uniformly mixing;
(3) and placing the agate ball milling tank on a ball mill for ball milling and purifying to obtain the porous magnesium silicate.
Has the advantages that: in the preparation process, the temperature rise and the heating are not needed, and the reaction is carried out after the solvent is dissolved into liquid.
Preferably, the method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) mixing 15-200 parts by weight of solid compound containing magnesium element with 60-240 parts by weight of sodium silicate solid, and pouring into an agate ball milling tank;
(2) putting 800 parts by weight of 200-800 parts of agate balls into the agate ball-milling tank in the step (1), and uniformly mixing;
(3) placing the agate ball milling tank on a ball mill for ball milling, wherein the ball milling rotation speed is 40-400rpm, reacting for 2-8h, and purifying to obtain the magnesium silicate.
Preferably, the purification comprises the steps of: and drying, grinding, cleaning, drying and grinding the ball-milled product to obtain the purified magnesium silicate.
Preferably, the drying temperature is 60 ℃.
Preferably, the solid compound containing magnesium is MgCl2、Mg(NO3)2、MgSO4、Mg(OH)2、4MgCO3·Mg(OH)2·4H2And one or more of O.
Preferably, the magnesium silicate has a structural general formula of MgxSiyOx+2y+zH2zWherein x is more than or equal to 2 and less than or equal to 5; y is more than or equal to 2 and less than or equal to 6; z is more than or equal to 1 and less than or equal to 4.
Preferably, the magnesium silicate has a specific surface area of 100-800m2·g-1。
The second technical problem to be solved by the present invention is to provide a magnesium silicate prepared by the above preparation method.
The invention solves the technical problems through the following technical means:
the magnesium silicate prepared by the preparation method has a general structural formula of MgxSiyOx+2y+zH2zWherein x is more than or equal to 2 and less than or equal to 5; y is more than or equal to 2 and less than or equal to 6; z is more than or equal to 1 and less than or equal to 4.
Has the advantages that: the magnesium silicate prepared by the invention has the specific surface area of 100-800m2·g-1The composite material has the excellent characteristics of large pore structure, large specific surface area and surface charge, and has good adsorption effect on organic dye and heavy metal ions. Wherein for Cu2+The adsorption rate of the adsorbent can reach 80%, the maximum adsorption capacity can also reach 223.05mg/g, and the maximum adsorption capacity for methylene blue can reach 300 mg/g.
Preferably, the magnesium silicate has a specific surface area of 100-800m2·g-1。
The invention also provides an application of the magnesium silicate prepared by the preparation method in adsorption of heavy metal ions.
Has the advantages that: the magnesium silicate prepared by the invention has better adsorption effect on heavy metal ions; wherein for Cu2+The adsorption rate of (2) can reach 80%, and the maximum adsorption quantity can also reach 223.05 mg/g.
Preferably, the heavy metal ion is Cu2+。
The fourth technical problem to be solved by the invention is to provide an application of the magnesium silicate prepared by the preparation method in adsorption of organic dye.
Has the advantages that: the magnesium silicate prepared by the invention has better adsorption effect on organic dye; wherein the maximum adsorption capacity of the methylene blue can reach 300 mg/g.
Preferably, the organic dye is methylene blue.
The invention has the advantages that:
(1) the preparation method is simple, does not need to be heated up in the preparation process, does not need a solvent to dissolve the raw materials into liquid and then carries out reaction, is energy-saving and environment-friendly, and is easy for large-scale application and large-scale industrial production;
(2) the ball milling method can fully convert the heat energy brought by high-speed rotation into reaction energy while mixing the raw materials, and improves the performance of the product magnesium silicate, and the specific surface area of the magnesium silicate prepared by the invention is 100-800m2·g-1The composite material has the excellent characteristics of large pore structure, large specific surface area and surface charge, and has good adsorption effect on organic dye and heavy metal ions; wherein for Cu2+The adsorption rate of the adsorbent can reach 80%, the maximum adsorption capacity can also reach 223.05mg/g, and the maximum adsorption capacity for methylene blue can reach 300 mg/g.
Drawings
FIG. 1 is an XRD spectrum of magnesium silicate in example 1 of the present invention;
FIG. 2 is an SEM photograph of magnesium silicate in example 1 of the present invention;
FIG. 3 is a BET adsorption/desorption graph of magnesium silicate prepared in example 1 of the present invention;
FIG. 4 is a BET pore size distribution chart of magnesium silicate prepared in example 1 of the present invention;
FIG. 5 shows that magnesium silicate absorbs Cu in the embodiment 1 of the present invention2+Adsorption rate graph of (a);
FIG. 6 shows that magnesium silicate absorbs Cu in the embodiment 1 of the present invention2+Adsorption capacity graph of (1);
FIG. 7 is a graph showing the adsorption amount of methylene blue by magnesium silicate produced in example 1 of the present invention;
FIG. 8 is an XRD spectrum of a product obtained by a comparative example of the present invention;
FIG. 9 is a BET adsorption/desorption graph of a product obtained by a comparative example of the present invention;
FIG. 10 is a BET pore size distribution plot of a product made by a comparative example of the present invention;
FIG. 11 shows a product obtained by comparative example of the present invention vs. Cu2+Adsorption rate graph of (a);
FIG. 12 is a graph showing the product obtained in comparative example of the present invention vs. Cu2+Adsorption amount of (c).
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
A method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) 63g of MgNO are weighed3·6H2O solids and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 400g of agate balls into the agate ball milling tank in the step (1), and uniformly mixing, wherein the mass of the small balls in the agate balls accounts for 30%, the mass of the large balls accounts for 20%, the mass of the medium balls accounts for 50%, and the treatment of the other three agate ball milling tanks is the same; wherein the diameter D of the pelletsSmallThe diameter D of the medium ball is less than or equal to 0.5cm and less than 0.5cmInLess than 1cm, large sphere diameter DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to be 100rpm and the ball milling time to be 4 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) putting the dried sample in the step (4) into a powder grinding machine for grinding, adding deionized water into the ground sample, then putting the sample into a centrifugal cylinder, and carrying out centrifugal cleaning until the pH value of the solution is 6-8;
(6) and (3) drying the cleaned sample in a drying oven at 60 ℃, putting the dried sample into a powdering machine, and performing powdering and grinding again to obtain magnesium silicate powder.
The determination method comprises the following steps: the magnesium silicate powder thus obtained was subjected to X-ray diffraction (XRD) analysis, scanning electron microscope observation (SEM), BET specific surface area measurement, and Cu analysis2+The adsorption performance of (b) is measured; and (3) performing ultraviolet spectrophotometer measurement on the adsorption performance of the methylene blue, wherein XRD, SEM and BET measurement methods are the prior art.
For Cu2+The adsorption performance measurement of (1) comprises the following steps:
(1) 50ml of a copper ion solution (50 ppm) was charged into an Erlenmeyer flask, 10mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals of time, and the clear solution was taken out by filtration through a syringe and an organic filter.
(2) ICP measurements were performed on copper ions in the clear solution.
And (3) measuring results: as shown in FIG. 1, it is clear from the XRD pattern and the peak position thereof that the product obtained is porous magnesium silicate 2 MgO.3SiO2·H2O, as shown in FIG. 2, it can be seen from the SEM image that the prepared magnesium silicate powder is small in particle size and porous; as shown in FIG. 3, it can be seen from the BET test that the specific surface area of the magnesium silicate powder is 369m2In terms of/g, the mean pore diameter is 4.13 nm.
The ICP experiment showed that the adsorption of copper ions continued and gradually increased with time as shown in FIG. 4, the maximum adsorption amount was 150mg/g, and the adsorption rate was 60%.
The method for measuring the methylene blue adsorption performance of the organic dye comprises the following steps:
50ml of a 200ppm methylene blue solution was added to an Erlenmeyer flask, 32.5mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals, and the clear solution was taken out by filtration through a syringe and an organic filter head. As shown in FIG. 7, the maximum adsorption amount of magnesium silicate produced in this example to a methylene blue solution was 260 mg/g.
Example 2
A method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) 52g of MgCl were weighed2·6H2O solids and 71.62g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 400g of agate balls into the agate ball milling tank in the step (1), and uniformly mixing, wherein the mass of the medium and small agate balls accounts for 30%, the mass of the large agate balls accounts for 20%, and the mass of the medium agate balls accounts for 50%; the other three agate ball milling tanks are treated identically; wherein DSmall≤0.5cm，0.5cm＜DIn＜1cm，DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to be 200rpm and the ball milling time to be 3 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) putting the dried sample in the step (4) into a powder grinding machine for grinding, adding deionized water into the ground sample, then putting the sample into a centrifugal cylinder, and carrying out centrifugal cleaning until the pH value of the solution is 6-8;
(6) and (3) drying the cleaned sample in a drying oven at 60 ℃, putting the dried sample into a powdering machine, and performing powdering and grinding again to obtain magnesium silicate powder.
The determination method comprises the following steps: the magnesium silicate powder thus obtained was subjected to X-ray diffraction (XRD) analysis, scanning electron microscope observation (SEM), BET specific surface area measurement, and Cu analysis2+The adsorption performance of (b) is measured; and (3) performing ultraviolet spectrophotometer measurement on the adsorption performance of the methylene blue, wherein XRD, SEM and BET measurement methods are the prior art.
For Cu2+The adsorption performance measurement of (1) comprises the following steps:
(1) 50ml of a copper ion solution (50 ppm) was charged into an Erlenmeyer flask, 10mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals of time, and the clear solution was taken out by filtration through a syringe and an organic filter.
(2) ICP measurements were performed on copper ions in the clear solution.
And (3) measuring results: the product prepared in this example is porous magnesium silicate 2 MgO.3SiO2·H2And O. The BET test shows that the specific surface area of the magnesium silicate powder is 323m2In terms of/g, the mean pore diameter is 5.12 nm.
The ICP test result shows that the adsorption of the copper ions is continuously carried out and gradually increases along with the time, the maximum adsorption amount is 171mg/g, and the adsorption rate is 65%.
The method for measuring the methylene blue adsorption performance of the organic dye comprises the following steps:
50ml of a 200ppm methylene blue solution was added to an Erlenmeyer flask, 32.5mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals, and the clear solution was taken out by filtration through a syringe and an organic filter head.
The maximum adsorption amount of the magnesium silicate prepared in this example to a methylene blue solution was 280 mg/g.
Example 3
A method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) 60g of MgSO are weighed4·7H2O solids and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 300g of agate balls into the agate ball milling tank in the step (1), and uniformly mixing, wherein the mass of the medium and small agate balls accounts for 30%, the mass of the large agate balls accounts for 20%, and the mass of the medium agate balls accounts for 50%; the other three agate ball milling tanks are treated identically; wherein DSmall≤0.5cm，0.5cm＜DIn＜1cm，DBig (a)≥1cm；
(3) Covering the agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to 250rpm for 3.5 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) putting the dried sample in the step (4) into a powder grinding machine for grinding, adding deionized water into the ground sample, then putting the sample into a centrifugal cylinder, and carrying out centrifugal cleaning until the pH value of the solution is 6-8;
(6) and (3) drying the cleaned sample in a drying oven at 60 ℃, putting the dried sample into a powdering machine, and performing powdering and grinding again to obtain magnesium silicate powder.
The determination method comprises the following steps: the magnesium silicate powder thus obtained was subjected to X-ray diffraction (XRD) analysis, scanning electron microscope observation (SEM), BET specific surface area measurement, and Cu analysis2+The adsorption performance of (b) is measured; performing ultraviolet spectrophotometer measurement on the adsorption performance of methylene blue, wherein the XRD, SEM and BET measurement methods are the conventional methodsProvided is a technique.
For Cu2+The adsorption performance measurement of (1) comprises the following steps:
(1) 50ml of a copper ion solution (50 ppm) was charged into an Erlenmeyer flask, 10mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals of time, and the clear solution was taken out by filtration through a syringe and an organic filter.
(2) ICP measurements were performed on copper ions in the clear solution.
And (3) measuring results: as is clear from the XRD pattern and the position of its peak, the product prepared is porous magnesium silicate. As can be seen from the SEM image, the prepared magnesium silicate powder has a small particle size and is porous. As can be seen from the BET test, the specific surface area of the magnesium silicate powder was 402m2In terms of/g, the mean pore diameter was 3.36 nm.
The ICP test result shows that the adsorption of the copper ions is continuously carried out and gradually increases along with the time, the maximum adsorption amount is 129mg/g, and the adsorption rate is 53%.
The method for measuring the methylene blue adsorption performance of the organic dye comprises the following steps:
50ml of a 200ppm methylene blue solution was added to an Erlenmeyer flask, 32.5mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals, and the clear solution was taken out by filtration through a syringe and an organic filter head.
The maximum adsorption amount of the magnesium silicate prepared in this example to a methylene blue solution was 230 mg/g.
Example 4
A method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) 16g of Mg (OH) were weighed2Solid and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) 300g of agate balls are put into the agate ball milling pot in the step (1) and mixedThe mixture is uniform, wherein the mass of the medium and small balls in the agate balls accounts for 30%, the mass of the large balls accounts for 20%, and the mass of the medium balls accounts for 50%; the other three agate ball milling tanks are treated identically; wherein DSmall≤0.5cm，0.5cm＜DIn＜1cm，DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to 400rpm for 6 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) putting the dried sample in the step (4) into a powder grinding machine for grinding, adding deionized water into the ground sample, then putting the sample into a centrifugal cylinder, and carrying out centrifugal cleaning until the pH value of the solution is 6-8;
(6) and (3) drying the cleaned sample in a drying oven at 60 ℃, putting the dried sample into a powdering machine, and performing powdering and grinding again to obtain magnesium silicate powder.
The determination method comprises the following steps: the magnesium silicate powder thus obtained was subjected to X-ray diffraction (XRD) analysis, scanning electron microscope observation (SEM), BET specific surface area measurement, and Cu analysis2+The adsorption performance of (b) is measured; and (3) performing ultraviolet spectrophotometer measurement on the adsorption performance of the methylene blue, wherein XRD, SEM and BET measurement methods are the prior art.
For Cu2+The adsorption performance measurement of (1) comprises the following steps:
(1) 50ml of a copper ion solution (50 ppm) was charged into an Erlenmeyer flask, 10mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals of time, and the clear solution was taken out by filtration through a syringe and an organic filter.
(2) ICP measurements were performed on copper ions in the clear solution.
And (3) measuring results: as is clear from the XRD pattern and the position of its peak, the product prepared is porous magnesium silicate. As can be seen from the SEM image, the prepared magnesium silicate powder has a small particle size and is porous. The BET test shows that the specific surface area of the magnesium silicate powder is 456m2In terms of a/g, the mean pore diameter is 2.98 nm.
The ICP test result shows that the adsorption of the copper ions is continuously carried out and gradually increases along with the time, the maximum adsorption amount is 110mg/g, and the adsorption rate is 47%.
The method for measuring the methylene blue adsorption performance of the organic dye comprises the following steps:
50ml of a 200ppm methylene blue solution was added to an Erlenmeyer flask, 32.5mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals, and the clear solution was taken out by filtration through a syringe and an organic filter head.
The maximum adsorption amount of magnesium silicate prepared in this example to a methylene blue solution was 205 mg/g.
Example 5
A method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) 24g of 4MgCO are weighed3·Mg(OH)2·4H2O solids and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 300g of agate balls into the agate ball milling tank in the step (1), and uniformly mixing, wherein the mass of the medium and small agate balls accounts for 30%, the mass of the large agate balls accounts for 20%, and the mass of the medium agate balls accounts for 50%; the treatment of the rest agate ball milling tanks is the same; wherein DSmall≤0.5cm，0.5cm＜DIn＜1cm，DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to be 200rpm and the ball milling time to be 6 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) putting the dried sample in the step (4) into a powder grinding machine for grinding, adding deionized water into the ground sample, then putting the sample into a centrifugal cylinder, and carrying out centrifugal cleaning until the pH value of the solution is 6-8;
(6) and (3) drying the cleaned sample in a drying oven at 60 ℃, putting the dried sample into a powdering machine, and performing powdering and grinding again to obtain magnesium silicate powder.
The determination method comprises the following steps: the magnesium silicate powder thus obtained was subjected to X-ray diffraction (XRD) analysis, scanning electron microscope observation (SEM), BET specific surface area measurement, and Cu analysis2+The adsorption performance of (b) is measured; and (3) performing ultraviolet spectrophotometer measurement on the adsorption performance of the methylene blue, wherein XRD, SEM and BET measurement methods are the prior art.
For Cu2+The adsorption performance measurement of (1) comprises the following steps:
(1) 50ml of a copper ion solution (50 ppm) was charged into an Erlenmeyer flask, 10mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals of time, and the clear solution was taken out by filtration through a syringe and an organic filter.
(2) ICP measurements were performed on copper ions in the clear solution.
And (3) measuring results: as is clear from the XRD pattern and the position of its peak, the product prepared is porous magnesium silicate. As can be seen from the SEM image, the prepared magnesium silicate powder has a small particle size and is porous. The BET test shows that the specific surface area of the magnesium silicate powder is 384m2In terms of a/g, the mean pore diameter is 4.01 nm.
The ICP test result shows that the adsorption of the copper ions is continuously carried out and gradually increases along with the time, the maximum adsorption amount is 145mg/g, and the adsorption rate is 58%.
The method for measuring the methylene blue adsorption performance of the organic dye comprises the following steps:
50ml of a 200ppm methylene blue solution was added to an Erlenmeyer flask, 32.5mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals, and the clear solution was taken out by filtration through a syringe and an organic filter head.
The maximum adsorption amount of magnesium silicate prepared in this example to a methylene blue solution was 247 mg/g.
Example 6
A method for preparing porous magnesium silicate by using a ball milling method comprises the following steps:
(1) 20g of MgCl were weighed2、Mg(NO3)2、MgSO4Solid and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 300g of agate balls into the agate ball milling tank in the step (1), and uniformly mixing, wherein the mass of the medium and small agate balls accounts for 30%, the mass of the large agate balls accounts for 20%, and the mass of the medium agate balls accounts for 50%; the treatment of the rest agate ball milling tanks is the same; wherein DSmall≤0.5cm，0.5cm＜DIn＜1cm，DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to 250rpm for 8 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) putting the dried sample in the step (4) into a powder grinding machine for grinding, adding deionized water into the ground sample, then putting the sample into a centrifugal cylinder, and carrying out centrifugal cleaning until the pH value of the solution is 6-8;
(6) and (3) drying the cleaned sample in a drying oven at 60 ℃, putting the dried sample into a powdering machine, and performing powdering and grinding again to obtain magnesium silicate powder.
The determination method comprises the following steps: the magnesium silicate powder thus obtained was subjected to X-ray diffraction (XRD) analysis, scanning electron microscope observation (SEM), BET specific surface area measurement, and Cu analysis2+The adsorption performance of (b) is measured; and (3) performing ultraviolet spectrophotometer measurement on the adsorption performance of the methylene blue, wherein XRD, SEM and BET measurement methods are the prior art.
For Cu2+The adsorption performance measurement of (1) comprises the following steps:
(1) 50ml of a copper ion solution (50 ppm) was charged into an Erlenmeyer flask, 10mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals of time, and the clear solution was taken out by filtration through a syringe and an organic filter.
(2) ICP measurements were performed on copper ions in the clear solution.
And (3) measuring results: as is clear from the XRD pattern and the position of its peak, the product prepared is porous magnesium silicate. As can be seen from the SEM image, the prepared magnesium silicate powder has a small particle size and is porous. The BET test shows that the specific surface area of the magnesium silicate powder is 780m2In terms of/g, the mean pore diameter is 10.12 nm.
The ICP test result shows that the adsorption of the copper ions is continuously carried out and gradually increases along with the time, the maximum adsorption amount is 223.05mg/g, and the adsorption rate is 89%.
The method for measuring the methylene blue adsorption performance of the organic dye comprises the following steps:
50ml of a 200ppm methylene blue solution was added to an Erlenmeyer flask, 32.5mg of the solid powder of magnesium silicate prepared in this example was added to the solution, the mixture was shaken in a shaker at a temperature of 20 ℃ and a speed of 160r/min, and the sampling was carried out at intervals, and the clear solution was taken out by filtration through a syringe and an organic filter head.
The maximum adsorption amount of the magnesium silicate prepared in this example to a methylene blue solution was 300 mg/g.
Comparative example 1
This comparative example differs from example 1 in that: a centrifugal washing step is not included.
A process for preparing magnesium silicate comprising the steps of:
(1) 63g of MgNO are weighed3·6H2O solids and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 400g of agate balls into the agate ball milling pot in the step (1), and uniformly mixing, wherein the mass of the small balls in the agate balls accounts for 30%, the mass of the large balls accounts for 20%, the mass of the medium balls accounts for 50%, and the diameter D of the small ballsSmallThe diameter D of the medium ball is less than or equal to 0.5cm and less than 0.5cmInLess than 1cm, large sphere diameter DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to be 100rpm and the ball milling time to be 4 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) and (4) putting the dried sample in the step (4) into a powder grinding machine for grinding to obtain magnesium silicate powder.
The experimental results are as follows: as can be seen from FIGS. 8-12, the magnesium silicate obtained contains a large amount of sodium nitrate as an impurity, which affects the specific surface area and the average pore diameter of the magnesium silicate, and further affects the Cu content2+The adsorption of (b) has a negative effect.
Comparative example 2
This comparative example differs from example 1 in that: reduction of the mass of the raw material.
A process for preparing magnesium silicate comprising the steps of:
(1) 6.3g of MgNO are weighed3·6H2O solids and 8.626g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 400g of agate balls into the agate ball milling pot in the step (1), and uniformly mixing, wherein the mass of the small balls in the agate balls accounts for 30%, the mass of the large balls accounts for 20%, the mass of the medium balls accounts for 50%, and the diameter D of the small ballsSmallThe diameter D of the medium ball is less than or equal to 0.5cm and less than 0.5cmInLess than 1cm, large sphere diameter DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to be 100rpm and the ball milling time to be 4 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) and (4) putting the dried sample in the step (4) into a powder grinding machine for grinding to obtain magnesium silicate powder.
The adsorption of the obtained magnesium silicate powder to copper ions was continued and gradually increased with time, and the maximum adsorption amount was 50 mg/g.
Comparative example 3
This comparative example differs from example 1 in that: reduction in the mass of the agate ball.
A process for preparing magnesium silicate comprising the steps of:
(1) 63g of MgNO are weighed3·6H2O solids and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 100g of agate balls into the agate ball milling pot in the step (1), and uniformly mixing, wherein the mass of the small balls in the agate balls accounts for 30%, the mass of the large balls accounts for 20%, the mass of the medium balls accounts for 50%, and the diameter D of the small ballsSmallThe diameter D of the medium ball is less than or equal to 0.5cm and less than 0.5cmInLess than 1cm, large sphere diameter DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to be 100rpm and the ball milling time to be 4 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) and (4) putting the dried sample in the step (4) into a powder grinding machine for grinding to obtain magnesium silicate powder.
The adsorption of the obtained magnesium silicate powder to copper ions was continued and gradually increased with time, and the maximum adsorption amount was 60 mg/g.
Comparative example 4
This comparative example differs from example 1 in that: and increasing the rotating speed of the ball mill.
A process for preparing magnesium silicate comprising the steps of:
(1) 63g of MgNO are weighed3·6H2O solids and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 400g of agate balls into the agate ball milling pot in the step (1), and uniformly mixing, wherein the mass of the small balls in the agate balls accounts for 30%, the mass of the large balls accounts for 20%, the mass of the medium balls accounts for 50%, and the diameter D of the small ballsSmallThe diameter D of the medium ball is less than or equal to 0.5cm and less than 0.5cmInLess than 1cm, large sphere diameter DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to 600rpm for 4 hours;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) and (4) putting the dried sample in the step (4) into a powder grinding machine for grinding to obtain magnesium silicate powder.
The adsorption of copper ions by the obtained magnesium silicate powder was continued and gradually increased with time, and the maximum adsorption amount was 72 mg/g.
Comparative example 5
This comparative example differs from example 1 in that: shortening the ball milling time.
A process for preparing magnesium silicate comprising the steps of:
(1) 63g of MgNO are weighed3·6H2O solids and 86.26g of Na2SiO3·9H2Mixing the O solid, and pouring the mixture into an agate ball milling tank;
(2) putting 400g of agate balls into the agate ball milling pot in the step (1), and uniformly mixing, wherein the mass of the small balls in the agate balls accounts for 30%, the mass of the large balls accounts for 20%, the mass of the medium balls accounts for 50%, and the diameter D of the small ballsSmallThe diameter D of the medium ball is less than or equal to 0.5cm and less than 0.5cmInLess than 1cm, large sphere diameter DBig (a)≥1cm；
(3) Covering an agate ball milling tank with a cover, placing the agate ball milling tank on a ball mill for ball milling, and adjusting the rotating speed to be 100rpm and the ball milling time to be 0.5 h;
(4) taking out the ball-milled product, and drying in a 60 ℃ oven;
(5) and (4) putting the dried sample in the step (4) into a powder grinding machine for grinding to obtain magnesium silicate powder.
The adsorption of the obtained magnesium silicate powder to copper ions was continued and gradually increased with time, and the maximum adsorption amount was 25 mg/g.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for preparing porous magnesium silicate by using a ball milling method is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing a solid compound containing magnesium element with a sodium silicate solid, and pouring the mixture into an agate ball milling tank;
(2) placing agate balls into the agate ball milling tank in the step (1) and uniformly mixing;
(3) and placing the agate ball milling tank on a ball mill for ball milling and purifying to obtain the magnesium silicate.
2. The method for producing a porous magnesium silicate by a ball milling method according to claim 1, characterized in that: the method comprises the following steps:
(1) mixing 15-200 parts by weight of solid compound containing magnesium element with 60-240 parts by weight of sodium silicate solid, and pouring into an agate ball milling tank;
(2) putting 800 parts by weight of 200-800 parts of agate balls into the agate ball-milling tank in the step (1), and uniformly mixing;
(3) placing the agate ball milling tank on a ball mill for ball milling, wherein the ball milling rotation speed is 40-400rpm, reacting for 2-8h, and purifying to obtain the magnesium silicate.
3. The method for producing a porous magnesium silicate by a ball milling method according to claim 1, characterized in that: the purification comprises the following steps: and drying, grinding, cleaning, drying and grinding the ball-milled product to obtain the purified magnesium silicate.
4. The method for producing a porous magnesium silicate by a ball milling method according to claim 3, characterized in that: the drying temperature is 60 ℃.
5. The method for producing a porous magnesium silicate by a ball milling method according to claim 1, characterized in that: said magnesium-containingSolid compounds of elements MgCl2、Mg(NO3)2、MgSO4、Mg(OH)2、4MgCO3·Mg(OH)2·4H2And one or more of O.
6. The method for producing a porous magnesium silicate by a ball milling method according to claim 1, characterized in that: the magnesium silicate has a structural general formula of MgxSiyOx+2y+zH2zWherein x is more than or equal to 2 and less than or equal to 5; y is more than or equal to 2 and less than or equal to 6; z is more than or equal to 1 and less than or equal to 4.
7. The method for producing a porous magnesium silicate by a ball milling method according to claim 1, characterized in that: the specific surface area of the magnesium silicate is 100-800m2·g-1。
8. A magnesium silicate produced by the method for producing a porous magnesium silicate by a ball milling method according to any one of claims 1 to 7, characterized in that: the magnesium silicate has a structural general formula of MgxSiyOx+2y+zH2zWherein x is more than or equal to 2 and less than or equal to 5; y is more than or equal to 2 and less than or equal to 6; z is more than or equal to 1 and less than or equal to 4.
9. Use of a magnesium silicate obtained by the method for producing a porous magnesium silicate by ball milling according to any one of claims 1 to 7 for adsorbing heavy metal ions.
10. Use of magnesium silicate obtained by the method for preparing porous magnesium silicate by ball milling according to any one of claims 1 to 7 for adsorbing organic dyes.
CN202010041192.6A 2020-01-15 2020-01-15 Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate Withdrawn CN113120914A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010041192.6A CN113120914A (en) 2020-01-15 2020-01-15 Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010041192.6A CN113120914A (en) 2020-01-15 2020-01-15 Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate

Publications (1)

Publication Number Publication Date
CN113120914A true CN113120914A (en) 2021-07-16

Family

ID=76771319

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010041192.6A Withdrawn CN113120914A (en) 2020-01-15 2020-01-15 Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate

Country Status (1)

Country Link
CN (1) CN113120914A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115624951A (en) * 2022-10-31 2023-01-20 苏州北美国际高级中学 Cobalt ion rapid enrichment material and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101591177A (en) * 2009-06-19 2009-12-02 厦门大学 A kind of preparation method of magnesium silicate porous ceramic
US20130190163A1 (en) * 2012-01-20 2013-07-25 Tdk Corporation Dielectric ceramic and electronic component using the same
CN104760966A (en) * 2015-03-27 2015-07-08 中国地质大学（武汉） Method for mechanochemically synthesizing magnesium lithium silicate
CN106237975A (en) * 2016-08-09 2016-12-21 北京化工大学 A kind of high-ratio surface big pore volume adsorption of magnesium silicate material and its preparation method and application
CN107867836A (en) * 2016-09-23 2018-04-03 卢路平 A kind of Mg2SiO4The preparation method of microwave-medium ceramics

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101591177A (en) * 2009-06-19 2009-12-02 厦门大学 A kind of preparation method of magnesium silicate porous ceramic
US20130190163A1 (en) * 2012-01-20 2013-07-25 Tdk Corporation Dielectric ceramic and electronic component using the same
CN104760966A (en) * 2015-03-27 2015-07-08 中国地质大学（武汉） Method for mechanochemically synthesizing magnesium lithium silicate
CN106237975A (en) * 2016-08-09 2016-12-21 北京化工大学 A kind of high-ratio surface big pore volume adsorption of magnesium silicate material and its preparation method and application
CN107867836A (en) * 2016-09-23 2018-04-03 卢路平 A kind of Mg2SiO4The preparation method of microwave-medium ceramics

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
李清海等: "沉淀法与研磨法制备二氧化硅微粉的比较", 《材料与冶金学报》 *
杜鹏程等: "球磨工艺对Mg_2SiO_4合成及其粉碎粒度影响", 《中国陶瓷工业》 *
杨华明等: "超细粉碎机械化学的研究进展", 《中国粉体技术》 *
陈勇等: "镁橄榄石合成反应动力学研究", 《东北大学学报(自然科学版)》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115624951A (en) * 2022-10-31 2023-01-20 苏州北美国际高级中学 Cobalt ion rapid enrichment material and preparation method thereof

Similar Documents

Publication Publication Date Title
An et al. A study on the consecutive preparation of silica powders and active carbon from rice husk ash
Feng et al. Simultaneous reclaiming phosphate and ammonium from aqueous solutions by calcium alginate-biochar composite: Sorption performance and governing mechanisms
CN111203180B (en) Magnetic biochar composite adsorbent and preparation method and application thereof
Gao et al. Preparation of high surface area-activated carbon from lignin of papermaking black liquor by KOH activation for Ni (II) adsorption
Zou et al. Structure and adsorption properties of sewage sludge-derived carbon with removal of inorganic impurities and high porosity
CN108033448A (en) A kind of coconut husk-sludge composite activated carbon and its preparation method and application
CN106457235B (en) For the system and method from ardealite removal of impurity and manufacture gypsum adhesive and product
CN101492165A (en) Organic modification method for attapulgite stone and uses of organic modified attapulgite stone
CN107138131A (en) A kind of preparation method of the oxidation of coal aluminium composite material of efficient absorption Cr (VI)
CN112934168A (en) Magnesium-containing silica gel composite material and preparation method and application thereof
CN114425340A (en) Preparation of charcoal-modified cobalt-iron bimetallic composite catalyst and application of charcoal-modified cobalt-iron bimetallic composite catalyst in catalytic degradation of tetracycline
Ahmed et al. Characterization and application of kaolinite clay as solid phase extractor for removal of copper ions from environmental water samples
CN110394154B (en) Preparation method and application of moso bamboo charcoal/FeMn-LDH composite material
CN110496597A (en) Graphene oxide modified montmorillonoid composite adsorbing material and its preparation method and application
CN106865565A (en) A kind of flyash synthesizes the method for X-type zeolite
Kumar et al. Comparison of physical-and chemical-activated Jatropha curcas husk carbon as an adsorbent for the adsorption of Reactive Red 2 from aqueous solution
CN113120914A (en) Method for preparing porous magnesium silicate by ball milling method and prepared magnesium silicate
CN110898808B (en) Mechanochemical preparation method of sulfur-rich alkyne carbon material and application of sulfur-rich alkyne carbon material in heavy metal ion adsorption in aqueous solution
CN108928880A (en) A kind of processing method of the waste water containing radioactive element
CN116651489A (en) Magnetic modified three-dimensional flower-shaped N-Bi 2 O 2 CO 3 / g-C 3 N 4 Preparation method and application of photocatalytic material
CN116272875A (en) Medicine dreg modified biochar, preparation method and application thereof
CN108946860A (en) A kind of application of functionalization composite material in uranium-containing waste water processing
KR101563984B1 (en) Method for manufacturing adsorbent using waste paper sludge
Behera et al. Adsorptive removal of phosphate ions using leached sea nodule residue generated by the reduction–roasting ammoniacal leaching process
Abdullah et al. Rhodamine 6G removal from aqueous solution with coconut shell-derived nanomagnetic adsorbent composite (Cs-nmac): Isotherm and kinetic studies

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
WW01 Invention patent application withdrawn after publication

Application publication date: 20210716

WW01 Invention patent application withdrawn after publication