CN113929106A - Ultrasonic synthesis method of magnesium lithium silicate - Google Patents

Ultrasonic synthesis method of magnesium lithium silicate Download PDF

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CN113929106A
CN113929106A CN202111276368.7A CN202111276368A CN113929106A CN 113929106 A CN113929106 A CN 113929106A CN 202111276368 A CN202111276368 A CN 202111276368A CN 113929106 A CN113929106 A CN 113929106A
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magnesium
lithium
ultrasonic
synthesis method
solution
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陶卓奇
杜鹏举
严朝阳
崔旭
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Shaoxing Shangyu Jiehua Chemical Co ltd
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Shaoxing Shangyu Jiehua Chemical Co ltd
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates

Abstract

The invention discloses an ultrasonic synthesis method of magnesium lithium silicate, which comprises the following specific raw materials: silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride, wherein the specific steps in the synthetic process are as follows, S1: firstly, silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compounds are placed in water to form a suspension, and the temperature and the ultrasonic frequency are maintained, namely S2 and S3. The method comprises the steps of carrying out ultrasonic pretreatment on the solution during the compound fusion period by an ultrasonic synthesis method, heating the solution after dissolution, and then cooling, washing, drying and crushing the fused solution to obtain the magnesium lithium silicate product.

Description

Ultrasonic synthesis method of magnesium lithium silicate
Technical Field
The invention relates to the technical field of chemical industry, in particular to an ultrasonic synthesis method of magnesium lithium silicate.
Background
The magnesium lithium silicate has thickening property and thixotropy and strong adsorption capacity, so that the magnesium lithium silicate is very suitable for cosmetics, can properly improve viscosity, suspension property, viscosity retention property, moisture retention property, lubricity and the like, can enhance the adhesive force of the cosmetics and skin care products together with the adsorption performance, has the functions of preventing cracking, falling and sterilization, has cation exchange and adsorption performance, can react with fatty amine, quaternary ammonium salt and the like to achieve organization, can adsorb essence, pigment or enzyme preparation, enhances fragrance, reduces the bitter taste of medicaments and the like, and can be applied to the fields with high requirements on medicines, foods, particularly cosmetics, skin care products, cosmetics and the like with harsh requirements on skin feel, so that the magnesium lithium silicate is used more in daily life, has larger market demand, but is more complex in the synthesis process and can generate a plurality of pollutants, the synthesis cost is high, and the production cost of enterprises is increased, so that the ultrasonic synthesis method of the magnesium lithium silicate is provided.
Disclosure of Invention
Therefore, the invention aims to provide an ultrasonic synthesis method of magnesium lithium silicate, which is characterized in that the ultrasonic pretreatment is carried out on the solution during the compound fusion period by the ultrasonic synthesis method, the temperature is raised after the solution is dissolved, and then the fused solution is cooled, washed, dried and crushed to obtain the magnesium lithium silicate product.
To solve the above technical problem, according to an aspect of the present invention, the present invention provides the following technical solutions:
an ultrasonic synthesis method of magnesium lithium silicate comprises the following specific raw materials:
Figure BDA0003330046650000011
Figure BDA0003330046650000021
the synthesis process comprises the following specific steps:
s1: firstly, placing silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compound in water to form suspension, and keeping temperature and ultrasonic frequency;
s2: secondly, adding a sodium hydroxide solution into the formed suspension, adjusting the pH value, keeping the temperature, and performing high-frequency ultrasonic treatment;
s3: and transferring the suspension with the adjusted pH value into a hydrothermal kettle, heating for reaction, filtering the solution after the reaction to obtain colloidal solid, washing the solid with deionized water to a washing solution, controlling the pH value range, drying in a vacuum environment, and finally crushing to obtain the magnesium-lithium silicate compound.
As a preferable scheme of the ultrasonic synthesis method of magnesium lithium silicate, the temperature at which the silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride, and lithium chloride compound are dissolved in water is 10 to 80 ℃.
In a preferable embodiment of the ultrasonic synthesis method of magnesium lithium silicate according to the present invention, the PH adjustment range in the step S2 is controlled between 8 and 15, and the ultrasonic treatment is performed at high frequency for 3 to 7 hours.
In a preferable embodiment of the ultrasonic synthesis method of magnesium lithium silicate according to the present invention, the temperature rise range in the step S3 is controlled to 150 to 300 ℃, and the reaction time is 6 to 10 hours.
As a preferable embodiment of the ultrasonic synthesis method of magnesium lithium silicate according to the present invention, in the step S3, after washing and fixing with deionized water, the PH is controlled to be 7 to 9, the temperature in the vacuum environment is controlled to be 50 to 120 ℃, and drying is performed for 16 to 24 hours.
As a preferable scheme of the ultrasonic synthesis method of the magnesium lithium silicate, the ultrasonic frequency of the solution in the step S3 in a reaction kettle is 100 MHZ-200 MHZ, and the ambient pressure value is 1.0-2.0 MPa.
Compared with the prior art, the invention has the beneficial effects that: the method comprises the steps of carrying out ultrasonic pretreatment on a solution during the compound fusion period by an ultrasonic synthesis method, heating the solution after dissolution, cooling, washing, drying and crushing the fused solution to obtain the magnesium lithium silicate product, wherein the production method has the advantages of simple process, short production time, low energy consumption, no toxicity, no harm, no pollution, environmental protection, suitability for mass production, low production cost and suitability for popularization and use, when the method is used specifically, silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compounds are placed in water to form a suspension, the temperature and the ultrasonic frequency are kept, then a sodium hydroxide solution is added into the formed suspension, the pH value is adjusted, the temperature is kept, high-frequency ultrasonic treatment is carried out, the suspension after the pH value is adjusted is transferred to a hydrothermal kettle, and (3) heating for reaction, filtering the solution to obtain colloidal solid after reaction, washing the solid with deionized water to a washing solution, controlling the pH value range, drying in a vacuum environment, and finally crushing to obtain the magnesium-lithium silicate compound.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and detailed embodiments, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise. Wherein:
FIG. 1 is a flow chart of an ultrasonic synthesis method of magnesium lithium silicate of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described herein, and it will be apparent to those of ordinary skill in the art that the present invention may be practiced without departing from the spirit and scope of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Next, the present invention will be described in detail with reference to the drawings, and in the detailed description of the embodiments of the present invention, the cross-sectional views illustrating the structure of the device are not enlarged partially according to the general scale for convenience of illustration, and the drawings are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
The invention provides an ultrasonic synthesis method of magnesium lithium silicate, which comprises the steps of carrying out ultrasonic pretreatment on a solution during compound fusion by an ultrasonic synthesis method, heating after dissolution, and then cooling, washing, drying and crushing the fused solution to obtain a magnesium lithium silicate product.
Fig. 1 is a schematic view of an overall structure of an embodiment of an ultrasonic synthesis method of magnesium lithium silicate according to the present invention, and referring to fig. 1, specific raw materials of the ultrasonic synthesis method of magnesium lithium silicate according to the embodiment of the present invention include: silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride, and the concrete steps comprise: s1, S2, and S3.
Example 1:
an ultrasonic synthesis method of magnesium lithium silicate comprises the following specific raw materials:
Figure BDA0003330046650000051
the synthesis process comprises the following specific steps:
s1: firstly, when the temperature of a water body is controlled to be 10 ℃, silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compounds are placed in water to be fully stirred to form suspension, and the temperature and the ultrasonic frequency are kept;
s2: secondly, adding a sodium hydroxide solution into the formed suspension, adjusting the pH value to 8, keeping the temperature, and continuously performing high-frequency ultrasonic treatment with the frequency of 100MHZ for 3 hours;
s3: and transferring the suspension with the pH value adjusted to a hydrothermal kettle with the ambient pressure value of 1.0MPa, heating to 150 ℃ for treatment, reacting for 6 hours, filtering the solution after the reaction to obtain colloidal solid, washing the solid with deionized water to obtain a washing solution, controlling the pH value to be 7, continuously drying for 16 hours in a vacuum environment at the ambient temperature of 50 ℃, and finally crushing to obtain the magnesium lithium silicate compound.
Example 2:
an ultrasonic synthesis method of magnesium lithium silicate comprises the following specific raw materials:
Figure BDA0003330046650000061
the synthesis process comprises the following specific steps:
s1: firstly, when the temperature of a water body is controlled to be 60 ℃, silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compounds are placed in water to be fully stirred to form suspension, and the temperature and the ultrasonic frequency are kept;
s2: secondly, adding a sodium hydroxide solution into the formed suspension, adjusting the pH value to 12, keeping the temperature, and continuously performing high-frequency ultrasonic treatment with the frequency of 150MHZ for 5 hours;
s3: and transferring the suspension with the pH value adjusted to a hydrothermal kettle with the ambient pressure value of 1.5MPa, heating to 200 ℃ for treatment, wherein the reaction time is 8 hours, filtering the solution after the reaction to obtain colloidal solid, washing the solid with deionized water to washing liquid, controlling the pH value to be 8, continuously drying for 20 hours in a vacuum environment at the ambient temperature of 80 ℃, and finally crushing to obtain the magnesium-lithium silicate compound.
Example 3:
an ultrasonic synthesis method of magnesium lithium silicate comprises the following specific raw materials:
Figure BDA0003330046650000071
the synthesis process comprises the following specific steps:
s1: firstly, when the temperature of a water body is controlled to be 80 ℃, silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compounds are placed in water to be fully stirred to form suspension, and the temperature and the ultrasonic frequency are kept;
s2: secondly, adding a sodium hydroxide solution into the formed suspension, adjusting the pH value to 15, keeping the temperature, and continuously performing high-frequency ultrasonic treatment with the frequency of 200MHZ for 7 hours;
s3: and transferring the suspension with the pH value adjusted to a hydrothermal kettle with the ambient pressure value of 2.0MPa, heating to 300 ℃ for treatment, reacting for 10 hours, filtering the solution after the reaction to obtain colloidal solid, washing the solid with deionized water to obtain a washing solution, controlling the pH value to be 9, continuously drying for 24 hours in a vacuum environment at the ambient temperature of 120 ℃, and finally crushing to obtain the magnesium-lithium silicate compound.
Referring to fig. 1, in a specific use of the ultrasonic synthesis method of magnesium lithium silicate of the present embodiment, firstly, when a water temperature is controlled to be 10 to 80 ℃, silicic acid, silica, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride, and lithium chloride compound are placed in water and fully stirred to form a suspension, a temperature and an ultrasonic frequency are maintained, then, a sodium hydroxide solution is added to the formed suspension, a PH value is adjusted to be 8 to 15, the temperature is maintained, a high-frequency ultrasonic treatment with a frequency of 100MHZ to 200MHZ is continuously performed for 3 to 7 hours, the suspension after the PH value is adjusted is transferred to a hydrothermal kettle with an environmental pressure value of 1.0 to 2.0MPa, the temperature is increased to 150 to 300 ℃ for treatment, a reaction time is 6 to 10 hours, the solution is filtered to obtain a colloidal solid, washing the solid with deionized water to washing liquid, controlling the pH value to be 7-9, continuously drying for 16-24 hours in a vacuum environment at the ambient temperature of 50-120 ℃, finally crushing to obtain the magnesium-lithium silicate compound, performing ultrasonic pretreatment on the solution during the compound fusion period by an ultrasonic synthesis method, heating after dissolution, and then cooling, washing, drying and crushing the fused solution to obtain the magnesium-lithium silicate product.
While the invention has been described above with reference to an embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the various features of the disclosed embodiments of the invention may be used in any combination, provided that no structural conflict exists, and the combinations are not exhaustively described in this specification merely for the sake of brevity and resource conservation. Therefore, it is intended that the invention not be limited to the particular embodiments disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims (6)

1. An ultrasonic synthesis method of magnesium lithium silicate is characterized in that the specific raw materials comprise:
Figure FDA0003330046640000011
the synthesis process comprises the following specific steps:
s1: firstly, placing silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compound in water to form suspension, and keeping temperature and ultrasonic frequency;
s2: secondly, adding a sodium hydroxide solution into the formed suspension, adjusting the pH value, keeping the temperature, and performing high-frequency ultrasonic treatment;
s3: and transferring the suspension with the adjusted pH value into a hydrothermal kettle, heating for reaction, filtering the solution after the reaction to obtain colloidal solid, washing the solid with deionized water to a washing solution, controlling the pH value range, drying in a vacuum environment, and finally crushing to obtain the magnesium-lithium silicate compound.
2. The ultrasonic synthesis method of magnesium lithium silicate according to claim 1, wherein the temperature for dissolving silicic acid, silicon dioxide, white carbon black, water glass, potassium silicate, magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium chloride, magnesium nitrate, lithium carbonate, lithium fluoride and lithium chloride compound in water is 10-80 ℃.
3. The ultrasonic synthesis method of lithium magnesium silicate according to claim 2, wherein the pH value adjustment range in the step S2 is controlled between 8 and 15, and the ultrasonic treatment is carried out for 3 to 7 hours at high frequency.
4. The ultrasonic synthesis method of lithium magnesium silicate according to claim 3, wherein the temperature rise range in the step of S3 is controlled to be 150-300 ℃, and the reaction time is 6-10 hours.
5. The ultrasonic synthesis method of lithium magnesium silicate according to claim 4, wherein the pH range of the fixed solution washed with ionized water in the step S3 is controlled to be 7-9, the temperature in the vacuum environment is controlled to be 50-120 ℃, and the solution is dried for 16-24 hours.
6. The ultrasonic synthesis method of lithium magnesium silicate according to claim 5, wherein the ultrasonic frequency of the solution in the reaction kettle in the step S3 is 100 MHZ-200 MHZ, and the ambient pressure value is 1.0-2.0 MPa.
CN202111276368.7A 2021-10-29 2021-10-29 Ultrasonic synthesis method of magnesium lithium silicate Pending CN113929106A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1993011069A1 (en) * 1991-11-30 1993-06-10 Laporte Industries Limited Synthesis of smectite clay minerals
CN106276931A (en) * 2016-08-01 2017-01-04 福建华夏蓝新材料科技有限公司 A kind of microwave synthesis method of lithium magnesium silicate
CN106745013A (en) * 2016-12-27 2017-05-31 江南大学 A kind of lithium magnesium silicate compound and preparation method thereof
CN112777603A (en) * 2021-01-29 2021-05-11 三棵树(上海)新材料研究有限公司 Hydrothermal synthesis method of magnesium lithium silicate with easy dispersion and excellent thickening performance

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1993011069A1 (en) * 1991-11-30 1993-06-10 Laporte Industries Limited Synthesis of smectite clay minerals
CN106276931A (en) * 2016-08-01 2017-01-04 福建华夏蓝新材料科技有限公司 A kind of microwave synthesis method of lithium magnesium silicate
CN106745013A (en) * 2016-12-27 2017-05-31 江南大学 A kind of lithium magnesium silicate compound and preparation method thereof
CN112777603A (en) * 2021-01-29 2021-05-11 三棵树(上海)新材料研究有限公司 Hydrothermal synthesis method of magnesium lithium silicate with easy dispersion and excellent thickening performance

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