CN115849396A - Preparation method of magnesium silicate and derivatives thereof - Google Patents

Preparation method of magnesium silicate and derivatives thereof Download PDF

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Publication number
CN115849396A
CN115849396A CN202310124602.7A CN202310124602A CN115849396A CN 115849396 A CN115849396 A CN 115849396A CN 202310124602 A CN202310124602 A CN 202310124602A CN 115849396 A CN115849396 A CN 115849396A
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magnesium silicate
derivatives
reaction
derivative
silicate
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CN202310124602.7A
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周小艺
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Abstract

The application provides a preparation method of magnesium silicate and derivatives thereof, and relates to the technical field of chemical industry. Mixing magnesium sulfate, sodium silicate and aluminum sulfate, adding water to prepare a solution, and removing excessive impurities after the reaction is finished to obtain magnesium silicate and a precursor of a derivative thereof; dissolving sodium pyrophosphate and sodium borate in water, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.1-0.5 h, transferring into a reaction kettle, cooling after the reaction is finished, taking out and drying to obtain the magnesium silicate and the derivative thereof. The magnesium silicate and the derivatives thereof can be artificially synthesized in the preparation process, the step of regulating the pH value is omitted, the preparation method is simpler, the cost is saved, and the pollution caused by waste acid or waste alkali can be avoided.

Description

Preparation method of magnesium silicate and derivatives thereof
Technical Field
The application relates to the technical field of chemical industry, in particular to a preparation method of magnesium silicate and derivatives thereof.
Background
The magnesium silicate and the derivatives thereof have good dispersibility, suspensibility, thickening property and thixotropy, are widely applied to important chemical fields of coatings, toothpastes, cosmetics, printing ink and the like, and have wide development and application prospects.
Although the natural magnesium silicate and the derivative ore thereof have low mining cost, the natural magnesium silicate and the derivative ore thereof contain a large amount of impurities inside, and the use requirement of high-end products cannot be met. Therefore, in actual use, people usually adopt artificially synthesized products to replace natural ores.
In the process of artificial synthesis, acid or alkali is usually added to adjust the pH value, the steps are complex, the cost is increased, and pollution is also caused.
Disclosure of Invention
The application aims to provide a preparation method of magnesium silicate and derivatives thereof, which selects a proper magnesium source, a silicon source and a modified compound as raw materials, does not need to additionally add a pH regulator, can also artificially synthesize the magnesium silicate and the derivatives thereof, omits a step of regulating the pH value, not only simplifies the preparation method, but also saves the cost, and can avoid pollution caused by waste acid or waste alkali.
The technical problem to be solved by the application is solved by adopting the following technical scheme.
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate, adding water to prepare a solution, and removing redundant impurities after the reaction is finished to obtain magnesium silicate and a precursor of a derivative thereof;
and B: dissolving sodium pyrophosphate and sodium borate in water, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.1-0.5 h, transferring into a reaction kettle, cooling after the reaction is finished, taking out and drying to obtain the magnesium silicate and the derivative thereof.
Compared with the prior art, the embodiment of the application has at least the following advantages or beneficial effects:
the embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which can enable a system to reach a proper pH value range by selecting proper magnesium sources, silicon sources and modified compounds as raw materials and regulating and controlling the proportion among the raw materials.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate, adding water to prepare a solution, and removing redundant impurities after the reaction is finished to obtain magnesium silicate and a precursor of a derivative thereof;
and B: dissolving sodium pyrophosphate and sodium borate in water, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.1-0.5 h, transferring into a reaction kettle, cooling after the reaction is finished, taking out and drying to obtain the magnesium silicate and the derivative thereof.
In some embodiments of the present application, the mass ratio of magnesium sulfate, sodium silicate, and aluminum sulfate is (4-5): (5-6): (1-2). The proper proportion is beneficial to better forming magnesium silicate and a precursor of a derivative thereof, and provides a good foundation for subsequent reaction. Meanwhile, the mass ratio of the magnesium sulfate, the sodium silicate and the aluminum sulfate directly influences the pH value in the system, and the proper proportion can provide a foundation for no addition of a pH regulator in the subsequent reaction.
In some embodiments herein, step a, the reaction conditions are 60 ℃ to 80 ℃, stirring for 6h to 8h. The magnesium silicate and the precursor of the derivative thereof are formed by continuously stirring at a lower temperature, the process is simple, and the reaction conditions are not harsh.
In some embodiments herein, step a provides a solids content of > 15% of magnesium silicate and its derivative precursors.
In some embodiments of the present application, in step B, the ratio of sodium pyrophosphate to sodium borate is 1: (1.2-1.5) mixing. The aqueous solution of sodium pyrophosphate and sodium borate is alkaline and is matched according to a certain proportion, and no additional pH regulator is needed.
In some embodiments of the present application, the solids content of the emulsion in step B is > 10%. The gel is easy to agglomerate in the later period when the solid content is too high, and the gel is not easy to form when the solid content is too low.
In some embodiments of the present application, the reaction conditions in the reaction vessel in step B are: 180-300 ℃ for 18-24 h. In a closed reaction kettle, a relatively high-temperature and high-pressure reaction environment is created by heating and pressurizing a reaction system, so that substances which are usually insoluble or insoluble are dissolved and recrystallized to carry out inorganic synthesis and material treatment. In hydrothermal reaction, water has multiple functions, not only serves as a solvent and simultaneously serves as a chemical component to participate in reaction, but also is a medium for transferring pressure, and crystals are rapidly formed and grown by controlling physical and chemical factors and accelerating reaction permeation. The process is simple, and the product with complete crystal form, uniform particle size distribution and good dispersibility can be obtained without high-temperature treatment, so that the energy consumption is relatively reduced.
The features and properties of the present application are described in further detail below with reference to examples.
Example 1
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4;
and B, step B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.2 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.5h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and (3) cooling, taking out and drying at 180 ℃ for 24h after the reaction is finished to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the magnesium silicate and its derivative precursor is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 2
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 5;
and B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.5 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the magnesium silicate derivative to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.4h, and transferring to a reaction kettle under the reaction conditions that: and (3) cooling, taking out and drying after the reaction is finished at 300 ℃ for 18h to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 3
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.5;
and B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.2 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.3h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and cooling, taking out and drying after the reaction is finished at 250 ℃ for 24h to obtain the magnesium silicate and the derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 4
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.5;
and B, step B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.3 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.2h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and (4) cooling at 280 ℃ for 22h after the reaction is finished, taking out and drying to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 5
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.7, adding water to prepare a solution, stirring for 8 hours at 65 ℃, and removing redundant impurities after the reaction is finished to obtain magnesium silicate and a precursor of a derivative thereof;
and B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.4 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.1-0.5 h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and (3) cooling, taking out and drying at 200 ℃ for 24h after the reaction is finished to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 6
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.3;
and B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.25 mixing, dissolving in water, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.4h, and transferring to a reaction kettle, wherein the reaction conditions are as follows: at 260 ℃ for 22 hours, cooling, taking out and drying after the reaction is finished to obtain the magnesium silicate and the derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 7
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.1 to 5.9, adding water to prepare a solution, stirring for 8 hours at 65 ℃, and removing redundant impurities after the reaction is finished to obtain magnesium silicate and a precursor of a derivative thereof;
and B, step B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.45 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.1h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and (3) cooling, taking out and drying at 230 ℃ for 18h after the reaction is finished to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 8
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.2;
and B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.35 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.3h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and (3) cooling, taking out and drying at 270 ℃ for 20h after the reaction is finished to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the magnesium silicate and its derivative precursor is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 9
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.3;
and B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.35 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.2h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and (3) cooling at 290 ℃ for 24h after the reaction is finished, taking out and drying to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
Example 10
The embodiment of the application provides a preparation method of magnesium silicate and derivatives thereof, which comprises the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate according to a mass ratio of 4.5;
and B: sodium pyrophosphate and sodium borate are mixed according to a mass ratio of 1:1.2 mixing, adding water to dissolve, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.5h, and transferring into a reaction kettle, wherein the reaction conditions are as follows: and (3) cooling, taking out and drying at 210 ℃ for 24h after the reaction is finished to obtain magnesium silicate and derivatives thereof.
In step A, the solid content of the precursor of magnesium silicate or its derivative is more than 15%.
In step B, the solids content of the emulsion is > 10%.
In summary, the embodiments of the present application provide a method for preparing magnesium silicate and its derivatives, which can make a system reach a suitable pH range by selecting a suitable magnesium source, a silicon source, and a modified compound as raw materials and adjusting and controlling the ratio among the raw materials, and can also artificially synthesize magnesium silicate and its derivatives during the preparation process, thereby omitting the step of adjusting the pH, not only making the preparation method simpler, but also saving the cost, and avoiding the pollution caused by waste acid or waste alkali.
The embodiments described above are some, but not all embodiments of the present application. The detailed description of the embodiments of the present application is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. 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 application.

Claims (7)

1. The preparation method of magnesium silicate and derivatives thereof is characterized by comprising the following steps:
step A: mixing magnesium sulfate, sodium silicate and aluminum sulfate, adding water to prepare a solution, and removing redundant impurities after the reaction is finished to obtain magnesium silicate and a precursor of a derivative thereof;
and B, step B: dissolving sodium pyrophosphate and sodium borate in water, mixing with the magnesium silicate and the precursor of the derivative thereof to form emulsion, adding lithium hydroxide, continuously stirring and dispersing for 0.1-0.5 h, transferring into a reaction kettle, cooling after the reaction is finished, taking out and drying to obtain the magnesium silicate and the derivative thereof.
2. The method for preparing magnesium silicate and its derivatives as claimed in claim 1, wherein the mass ratio of magnesium sulfate, sodium silicate and aluminum sulfate is (4-5): (5-6): 1-2).
3. The process for preparing magnesium silicate and its derivatives as claimed in claim 1, wherein in said step A, the reaction is carried out at 60-80 ℃ for 6-8 h under stirring.
4. The process for producing magnesium silicate and derivatives thereof as claimed in claim 1, wherein the solid content of the precursor of magnesium silicate and derivatives thereof obtained in step A is > 15%.
5. The method for preparing magnesium silicate and derivatives thereof according to claim 1, wherein in the step B, the mass ratio of sodium pyrophosphate to sodium borate is 1: (1.2-1.5) mixing.
6. The process of preparing magnesium silicate and derivatives thereof according to claim 1 wherein in step B, the solids content of the emulsion is > 10%.
7. The process for preparing magnesium silicate and derivatives thereof according to claim 1, wherein in step B, the reaction conditions in the reaction kettle are as follows: 180-300 ℃ for 18-24 h.
CN202310124602.7A 2023-02-16 2023-02-16 Preparation method of magnesium silicate and derivatives thereof Withdrawn CN115849396A (en)

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CN202310124602.7A CN115849396A (en) 2023-02-16 2023-02-16 Preparation method of magnesium silicate and derivatives thereof

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Application Number Priority Date Filing Date Title
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Publications (1)

Publication Number Publication Date
CN115849396A true CN115849396A (en) 2023-03-28

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Application publication date: 20230328