CN114849673A - Method for preparing magnesium silicate adsorbent with high specific surface area - Google Patents
Method for preparing magnesium silicate adsorbent with high specific surface area Download PDFInfo
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Abstract
The invention provides a preparation method of a magnesium silicate adsorbent with high specific surface area, which is realized by reacting inorganic magnesium salt and inorganic silicate in aqueous solution, adding a template agent and carrying out a calcination process. The preparation method has simplified and efficient process steps, and is suitable for industrial large-scale production of the magnesium silicate adsorbent. Finally, the magnesium silicate adsorbent with high specific surface area and average pore diameter is obtained, compared with the magnesium silicate adsorbent prepared by a common method, the pore diameter, the pore volume and the specific surface area are greatly increased, and the product performance is greatly enhanced.
Description
Technical Field
The invention relates to the technical field of preparation of inorganic silicate materials, in particular to a preparation method of a magnesium silicate adsorbent.
Background
An adsorbent is a solid material that can remove certain components in a gaseous or liquid environment. The adsorbent should have some of the following properties: (1) has large specific surface area and developed pore structure; (2) the adsorbent has good chemical stability, and does not react with the adsorbate to generate new pollutants; (3) the material has strong directional adsorption capacity and also has strong requirement on mechanical property; (4) the manufacturing process is simpler and the manufacturing cost is lower. Magnesium silicate adsorbents are becoming one of the important adsorbents due to their developed pore structure, high specific surface area, strong ion exchange capacity and low price.
The magnesium silicate adsorption capacity generally depends on its pore structure parameters including specific surface area, pore size, pore volume, and the like. Magnesium silicate adsorbents obtained by different preparation methods have different structural parameters, and generally, magnesium silicate adsorbents with higher specific surface area and larger pore volume can show excellent adsorption performance. For example, as described in the article "research on the preparation and adsorption properties of porous magnesium silicate" by Zhao Chun Yan, patents CN1424253 and US2384563A, the magnesium silicate adsorbent is conventionally prepared by heating and stirring water-soluble magnesium salts such as magnesium nitrate and magnesium sulfate together with metal silicate (usually sodium silicate), and reacting and precipitating to obtain magnesium silicate.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a novel method for preparing a magnesium silicate adsorbent with a high specific surface area. The technical scheme of the invention is as follows:
a process for preparing magnesium silicate adsorbent features that the inorganic magnesium salt and inorganic silicate are reacted in aqueous solution and proper template agent is added.
Further, the preparation method comprises the following steps:
step 1: preparing an aqueous solution of the inorganic silicate to obtain a solution I;
step 2: adding the template agent into the first solution, and stirring for reaction to obtain a third solution;
and step 3: dissolving the inorganic magnesium salt in water to obtain a solution II;
and 4, step 4: adding the solution II into the solution III, and stirring for reaction;
and 5: filtering after the reaction is finished, washing the filter cake with water, collecting the filter cake, and drying;
step 6: and calcining the dried product to obtain the final product.
In the preparation method, the inorganic silicate solution is a sodium silicate solution.
S1 specifically includes: and adding water to dilute the inorganic silicate solution to obtain a solution I.
Further, the molar ratio of silicon dioxide to sodium oxide, referred to as modulus for short, in the inorganic silicate solution is in the range of 2.9-3.2.
In the step 2, the template agent is one or more of quaternary ammonium salt surfactants and polyether surfactants, such as cetyl trimethyl ammonium bromide, dodecyl trimethyl ammonium bromide, tetrabutyl ammonium bromide, cellulose polyether, polyethylene glycol ether, polypropylene glycol ether, glycerol polyether, random polyether with various molecular weights, block polyether with various molecular weights, and the like. The addition of the template agent can play a template role with inorganic silicate, inspire the formation of the pore structure of the adsorbent product, and directionally generate the pore structure, thereby effectively improving the specific surface area and the pore size of the adsorbent product. The total amount of the template agent is selected to be 1-15% of the mass of the solution.
In the above production method, the inorganic magnesium salt is at least one selected from magnesium sulfate, magnesium chloride and magnesium nitrate, preferably magnesium sulfate.
In the preparation method, the concentration of the second solution is 1.6-2.0 mol/L.
In the preparation method, the solution two is added into the solution three in the step 4, and the stirring reaction is carried out, wherein the specific control conditions are as follows: adding the inorganic magnesium salt solution in a sectional manner or dropwise, wherein the adding time is 10-40min, the reaction temperature is 60-100 ℃, and the reaction time is 90-180 min.
Preferably, in the step 4, the solution two is added into the solution three to be stirred for reaction, and the specific control conditions further include: the inorganic magnesium salt solution is added dropwise, the feeding time is 20-30min, the reaction temperature is 70-90 ℃, and the reaction time is 120-150 min.
In the above preparation method, the step 5 of washing the filter cake with water is to remove the residual ions, and the washing effect is determined by dropping the barium chloride analysis solution into the filtrate, and the washing with water can be stopped if no white turbid substance appears.
In the preparation method, the drying in the step 5 is heating drying or spray drying, the heating drying temperature is 80-120 ℃, and the air inlet temperature of the spray drying is 200-300 ℃. The purpose of this step is in order to remove the moisture in the product, and the drying mode does not have the influence to the final result, and the selection heating drying operation is more convenient.
In the preparation method, the calcination time in the calcination process in the step 6 is 2-5 h, and the calcination temperature is 400-600 ℃. The muffle furnace was selected as the calcination instrument in this experiment. During the calcination process, a large number of microporous hole walls with weak adsorption performance in the adsorbent product can be collapsed to form mesopores and macropores with relatively good adsorption performance, and finally the magnesium silicate adsorbent with high specific surface area can be obtained and has good adsorption performance.
Preferably, the calcination time in the step 6 is 3-5 h, and the calcination temperature is 500-550 ℃.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
the template agent is added and calcined on the basis of the ordinary synthesis process, so that the specific surface area, the pore diameter and the pore volume of the magnesium silicate adsorbent product are obviously improved, and the adsorption performance of the adsorbent is improved. The preparation method has simplified and efficient process steps, and is suitable for industrial large-scale production of the magnesium silicate adsorbent with high specific surface area.
Detailed Description
In the description of the present invention, it is to be noted that those whose specific conditions are not specified in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturers. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The technical solutions provided by the present invention will be clearly and completely described below with reference to specific embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example 1
The embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silica) of sodium silicate solution with modulus of 2.9:1, namely: the inorganic silicate solution is sodium silicate solution, wherein the molar ratio of silicon dioxide to sodium oxide is 2.9:1, 225ml of deionized water is added into the inorganic silicate solution and then the inorganic silicate solution is stirred;
then 6.79g of hexadecyl trimethyl ammonium bromide (template agent) is weighed and added into the sodium silicate solution;
adding 0.2mol of magnesium sulfate into 125ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 1.6 mol/L;
dropwise adding the magnesium sulfate solution into a sodium silicate solution containing a template agent under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 10 min; after the dropwise adding, heating to 70 ℃, keeping the reaction temperature at 70 ℃ and the reaction time at 180 min;
after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 80 ℃ to obtain magnesium silicate white powder;
putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating to 600 ℃ at a heating rate of 10 ℃/min, keeping the calcining temperature at 600 ℃, calcining for 2 hours, cooling to 100 ℃ after calcining, and taking out to obtain calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is measured to be 506m 2 The pore volume was 0.4807cc/g, and the average pore diameter was 4.117 nm.
Example 2:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 8.80g of 3000 molecular weight block polyether polyethylene glycol-polypropylene glycol-polyethylene glycol is weighed and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding a magnesium sulfate solution into a sodium silicate solution containing a template agent under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 30min, after the dropwise adding is finished, heating to 90 ℃, keeping the reaction temperature at 90 ℃, and reacting for 90 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 100 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, raising the temperature to 400 ℃ at the heating rate of 10 ℃/min, keeping the calcining temperature at 400 ℃, calcining for 2 hours, reducing the temperature to 100 ℃ after calcining, and taking out the calcined magnesium silicate powder to obtain the calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is measured to be 492m 2 The pore volume is 0.4757cc/g, and the average pore diameter is 4.445 nm.
Example 3:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 6.79g of 3000 molecular weight block polyether polyethylene glycol-polypropylene glycol-polyethylene glycol are weighed and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 20min, heating to 70 ℃ after the dropwise adding is finished, keeping the reaction temperature at 70 ℃ and the reaction time at 120 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 120 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, raising the temperature to 560 ℃ at a heating rate of 10 ℃/min, keeping the calcining temperature at 560 ℃, calcining for 5h, reducing the temperature to 100 ℃ after calcining, and taking out the calcined magnesium silicate powder to obtain the calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is 547m 2 The pore volume is 0.6454cc/g, and the average pore diameter is 5.432 nm.
Example 4:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 6.79g of 12000 molecular weight block polyether polyethylene glycol-polypropylene glycol-polyethylene glycol is weighed and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 30min, heating to 80 ℃ after the dropwise adding is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time at 140 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 120 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, raising the temperature to 540 ℃ at a heating rate of 10 ℃/min, keeping the calcining temperature at 540 ℃, calcining for 5 hours, and taking out the ceramic crucible after the calcining is finished and the temperature is reduced to 100 ℃ to obtain calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is determined to be 498m 2 The pore volume is 0.5282cc/g, and the average pore diameter is 4.721 nm.
Example 5:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 3.40g of 12000 molecular weight block polyether polyethylene glycol-polypropylene glycol-polyethylene glycol is weighed and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 24min, heating to 80 ℃ after the dropwise adding is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time at 140 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 110 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, raising the temperature to 550 ℃ at the heating rate of 10 ℃/min, keeping the calcining temperature at 550 ℃, calcining for 4 hours, reducing the temperature to 100 ℃ after calcining, and taking out the calcined magnesium silicate powder to obtain the calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is measured to be 510m 2 The pore volume is 0.5153cc/g, and the average pore diameter is 4.397 nm.
Example 6:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 6.79g of 12000 molecular weight block polyether polyethylene glycol-polypropylene glycol-polyethylene glycol is weighed and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, stirring to obtain a magnesium sulfate solution with the concentration of 2.0mol/L, dropwise adding the magnesium sulfate solution into a sodium silicate solution under stirring to obtain a reaction solution with the silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 25min, heating to 90 ℃ after the dropwise adding is finished, keeping the reaction temperature at 90 ℃, and reacting for 110 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 90 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating to 530 ℃ at a heating rate of 10 ℃/min, keeping the calcining temperature at 530 ℃, calcining for 3 hours, cooling to 100 ℃ after calcining, and taking out to obtain calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is determined to be 502m 2 The pore volume is 0.5304cc/g, and the average pore diameter is 4.808 nm.
Example 7:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 3.40g of hydroxyethyl cellulose is weighed and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 25min, heating to 80 ℃ after the dropwise adding is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time at 120 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 120 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, raising the temperature to 550 ℃ at the heating rate of 10 ℃/min, keeping the calcining temperature at 550 ℃, calcining for 3 hours, reducing the temperature to 100 ℃ after calcining, and taking out the calcined magnesium silicate powder to obtain the calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is 508m 2 The pore volume is 0.5002cc/g, and the average pore diameter is 4.190 nm.
Example 8:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 3.40g of 3000 molecular weight block polyether polyethylene glycol-polypropylene glycol-polyethylene glycol is weighed and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 20min, heating to 80 ℃ after the dropwise adding is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time at 100 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 100 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, raising the temperature to 550 ℃ at the heating rate of 10 ℃/min, keeping the calcining temperature at 550 ℃, calcining for 3 hours, reducing the temperature to 100 ℃ after calcining, and taking out the calcined magnesium silicate powder to obtain the calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is measured to be 589m 2 The pore volume is 0.5495cc/g, and the average pore diameter is 4.489 nm.
Example 9:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; weighing 3.40g of hexadecyl trimethyl ammonium bromide, and adding the hexadecyl trimethyl ammonium bromide into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 30min, heating to 80 ℃ after the dropwise adding is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time at 130 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 120 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, raising the temperature to 550 ℃ at the heating rate of 10 ℃/min, keeping the calcining temperature at 550 ℃, calcining for 3 hours, reducing the temperature to 100 ℃ after calcining, and taking out the calcined magnesium silicate powder to obtain the calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is measured to be 520m 2 The pore volume is 0.5276cc/g, and the average pore diameter is 4.077 nm.
Example 10:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; then 6.79g of hexadecyl trimethyl ammonium bromide is measured and added into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 27min, heating to 80 ℃ after the dropwise adding is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time at 150 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 120 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating to 570 ℃ at the heating rate of 10 ℃/min, keeping the calcination temperature at 570 ℃, calcining for 5 hours, cooling to 100 ℃ after calcination, and taking out to obtain calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is determined to be 590m 2 The pore volume is 0.5912cc/g, and the average pore diameter is 4.376 nm.
Example 11:
the embodiment provides a preparation method of a magnesium silicate adsorbent, which comprises the following specific steps:
taking 0.7mol (calculated by silicon dioxide) of sodium silicate solution with the modulus of 3.1:1, adding 400ml of deionized water into the sodium silicate solution, and stirring the mixture; measuring 13.58g of hexadecyl trimethyl ammonium bromide, and adding the hexadecyl trimethyl ammonium bromide into the sodium silicate solution; adding 0.2mol of magnesium sulfate into 100ml of deionized water, and stirring to obtain a magnesium sulfate solution with the concentration of 2.0 mol/L; dropwise adding the magnesium sulfate solution into the sodium silicate solution under stirring to obtain a reaction solution with a silicon-magnesium ratio of 3:1, wherein the dropwise adding time is 30min, heating to 80 ℃ after the dropwise adding is finished, keeping the reaction temperature at 80 ℃, and keeping the reaction time at 120 min; after the reaction is finished, washing with water, filtering, and heating and drying in an oven at 120 ℃ to obtain magnesium silicate white powder; putting the magnesium silicate powder into a ceramic crucible, putting the ceramic crucible into a muffle furnace, heating to 500 ℃ at a heating rate of 10 ℃/min, keeping the calcining temperature at 500 ℃, calcining for 3 hours, cooling to 110 ℃ after calcining, and taking out to obtain calcined white magnesium silicate powder.
The specific surface area of the magnesium silicate powder is 600m 2 The pore volume is 0.4709cc/g, and the average pore diameter is 4.071 nm.
Comparative example 1
According to the process described in example 1, the magnesium silicate powder produced by the reaction has a specific surface area of 438m, except that no template agent is added after the sodium silicate solution is prepared 2 The pore volume is 0.4945cc/g, and the average pore diameter is 3.710 nm.
Comparative example 2:
CN201880033613.1 patent uses sodium silicate and magnesium sulfate to acidify and react to prepare the adsorbent with the specific surface area of 480m 2 In terms of a/g, the mean pore diameter is 3.9 nm.
Comparative example 3:
in example 1 of patent US7247699B2, the magnesium silicate adsorbent is synthesized by feeding magnesium sulfate solution, sodium silicate solution and sulfuric acid solution simultaneously for reaction, and the specific surface area is 308m 2 /g。
The measurement results are shown in table 1.
TABLE 1 measurement results of magnesium silicate powders prepared in examples 1 to 11 and comparative examples 1 to 3
In conclusion, the preparation method for the magnesium silicate adsorbent with high specific surface area provided by the invention has an obvious effect on the improvement of the physical parameter performance, the adsorption performance of the prepared adsorbent is obviously improved compared with that of a common magnesium silicate adsorbent, and the production process is simplified and efficient.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a magnesium silicate adsorbent is characterized by comprising the following steps: by reacting inorganic magnesium salts with inorganic silicates in aqueous solution and adding suitable templates.
2. The method of claim 1, wherein: the method comprises the following steps:
s1: preparing an aqueous solution of the inorganic silicate to obtain a solution I;
s2: adding the template agent into the first solution, and stirring for reaction to obtain a third solution;
s3: dissolving the inorganic magnesium salt in water to obtain a solution II;
s4: adding the solution II into the solution III, and stirring for reaction;
s5: filtering after the reaction is finished, washing the filter cake with water, collecting the filter cake, and drying;
s6: and calcining the dried product to obtain the final product.
3. The production method according to claim 1 or 2, characterized in that: the inorganic silicate solution is a sodium silicate solution.
4. The production method according to claim 3, characterized in that: the molar ratio of silica to sodium oxide in the inorganic silicate solution is in the range of 2.9: 1-3.2: 1.
5. the production method according to claim 1 or 2, characterized in that: the template agent is one or more of quaternary ammonium salt surfactants and polyether surfactants, and comprises hexadecyl trimethyl ammonium bromide, dodecyl trimethyl ammonium bromide, tetrabutyl ammonium bromide, cellulose polyether, polyethylene glycol ether, polypropylene glycol ether, glycerol polyether, random polyether with various molecular weights and block polyether with various molecular weights, wherein the total dosage of the template agent is selected to be 1-15% of the three mass of the solution.
6. The production method according to claim 1 or 2, characterized in that: the inorganic magnesium salt is at least one selected from magnesium sulfate, magnesium chloride and magnesium nitrate, and the concentration of the second solution is 1.6-2.0 mol/L.
7. The method of claim 2, wherein: and in the S4, adding the solution II into the solution III, and stirring for reaction, wherein the specific control conditions are as follows: adding the inorganic magnesium salt solution in a sectional manner or dropwise, wherein the adding time is 10-40min, the reaction temperature is 60-100 ℃, and the reaction time is 90-180 min.
8. The method of claim 7, wherein: in the S4, adding the solution II into the solution III, and stirring for reaction, wherein the specific control conditions are as follows: the inorganic magnesium salt solution is added dropwise, the feeding time is 20-30min, the reaction temperature is 70-90 ℃, and the reaction time is 120-150 min.
9. The method of claim 2, wherein: the calcination time in the calcination process of S6 is 2-5 h, and the calcination temperature is 400-600 ℃.
10. The method of claim 2, wherein: the calcination time in the S6 is 3-5 h, and the calcination temperature is 500-550 ℃.
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| CN108821300A (en) * | 2018-08-06 | 2018-11-16 | 东北大学 | One kind preparing CaSiO by discarded silicon slag3Method |
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| CN108821300A (en) * | 2018-08-06 | 2018-11-16 | 东北大学 | One kind preparing CaSiO by discarded silicon slag3Method |
| CN110980750A (en) * | 2019-12-24 | 2020-04-10 | 福州大学 | Preparation method and application of mesoporous magnesium silicate |
| CN113694878A (en) * | 2021-08-27 | 2021-11-26 | 浙江皇马科技股份有限公司 | Preparation method and application of magnesium silicate adsorbent |
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