CN111620348A - Preparation method of sodium silicate for nano silicon dioxide - Google Patents
Preparation method of sodium silicate for nano silicon dioxide Download PDFInfo
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- CN111620348A CN111620348A CN202010573736.3A CN202010573736A CN111620348A CN 111620348 A CN111620348 A CN 111620348A CN 202010573736 A CN202010573736 A CN 202010573736A CN 111620348 A CN111620348 A CN 111620348A
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- 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
- C01B33/32—Alkali metal silicates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
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- 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
- C01B33/32—Alkali metal silicates
- C01B33/325—After-treatment, e.g. purification or stabilisation of solutions, granulation; Dissolution; Obtaining solid silicate, e.g. from a solution by spray-drying, flashing off water or adding a coagulant
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- 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
Abstract
The invention discloses a preparation method of sodium silicate for nano silicon dioxide, relating to the technical field of inorganic materials, wherein refined quartz sand is used as a preparation raw material of sodium silicate, so that the purification process of impurities is avoided, and the problem that the quality of the sodium silicate is influenced due to excessive impurities is solved; the invention also carries out surface modification on the sodium silicate, and utilizes the homemade cyclopropyl formamidine glutarate as a modifier, thereby improving the water solubility of the sodium silicate; meanwhile, the nano silicon dioxide further prepared by the prepared sodium silicate has the characteristics of small particle size and narrow particle size distribution range, so that the quality of the nano silicon dioxide is improved, and the application field of the nano silicon dioxide is widened.
Description
The technical field is as follows:
the invention relates to the technical field of inorganic materials, in particular to a preparation method of sodium silicate for nano silicon dioxide.
Background art:
sodium silicate, commonly known as sodium silicate, and its aqueous solution is commonly known as sodium silicateGlass with the chemical formula of Na2O.nSiO2Belongs to soluble inorganic silicate. Sodium silicate is the most valuable filler in the soap industry, acts as a building, preservative, foam stabilizing in synthetic detergents, and can also be used as a filler in paper making, as a binder in the foundry industry, and in the manufacture of silica gels and silica gels, and is also an important raw material for the production of silica.
The nano material has at least one dimension in the range of nano size in a three-dimensional space, has small size effect, surface effect and macroscopic quantum tunneling effect, thus showing a plurality of unique properties and having wide application prospects in catalysis, filtering, light absorption, medicines, magnetic media, new materials and the like.
Nanosilicas range in size from 1 to 100nm and therefore possess many unique properties such as optical properties against ultraviolet light, and enhance the resistance to ageing, strength and chemicals of other materials. The preparation raw material sodium silicate of the nano silicon dioxide generally has the problems of unstable modulus, high iron content, more impurities, low total solid content and the like, so that the produced nano silicon dioxide has unstable quality, large particle size and wide particle size distribution range, and therefore, the quality is poor and the use requirement is difficult to meet. Therefore, the quality of the raw material sodium silicate is controlled, so that high-quality nano silicon dioxide can be prepared.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a preparation method of sodium silicate for nano-silica, which improves the solubility of sodium silicate by performing surface modification treatment on sodium silicate prepared by melting reaction, and can further play a role in regulating and controlling the particle size and specific surface area of a product when the nano-silica is prepared from the sodium silicate.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
a preparation method of sodium silicate for nano silicon dioxide comprises the following preparation steps:
(1) mixing SiO2Mixing refined quartz sand with content over 99% and soda ash uniformly, feeding into horse-shoe flame kiln, and heating at high temperature in air atmosphereCalcining to perform a melting reaction, and after the reaction is finished, performing water quenching and drying to obtain a sodium silicate crude product;
(2) crushing the crude sodium silicate into particles, then sending the particles into a high-pressure reaction kettle, introducing high-temperature steam for dissolving, filtering after complete dissolution, and taking filtrate to obtain a pure sodium silicate product;
(3) adding glutaric acid and (Z) -N-hydroxycyclopropanecarboxamidine into water, heating and stirring, then dropwise adding concentrated sulfuric acid, keeping the temperature for reaction, adding ethyl acetate for extraction after the reaction is finished, taking an organic phase, concentrating to remove ethyl acetate, and carrying out column chromatography to obtain cyclopropanecarboxamidine glutarate;
(4) adding the methyl cyclopropaneamidine glutarate into the pure sodium silicate, mixing at high speed, concentrating to remove water, drying and crushing to obtain the sodium silicate.
Chemical reaction formula of cyclopropyl formamidine glutarate:
the mass ratio of the refined quartz sand to the soda ash is 2-3: 1.
The temperature of the melting reaction was 1450-.
The temperature of the high-temperature steam is 145-160 ℃, and the pressure is 0.4-0.6 MPa.
The mole ratio of glutaric acid to (Z) -N-hydroxycyclopropanecarboxamidine is 1: 2-2.05.
The temperature of the heat preservation reaction is 70-90 ℃.
The mass ratio of the pure sodium silicate to the cyclopropyl formamidine glutarate is 1: 0.05-0.2.
The chemical reaction formula of sodium silicate is: na (Na)2CO3+nSiO2→Na2O.nSiO2+CO2↑
Because the surface of the nano silicon dioxide has a large amount of active hydroxyl groups and strong hydrophilicity, the nano silicon dioxide is easy to form agglomerates or secondary aggregation, thereby generating the nano silicon dioxide with large particle size. Aiming at the problem, the prepared sodium silicate is subjected to surface modification treatment by utilizing the cyprocoamidine glutarate when the sodium silicate is prepared, so that the prepared sodium silicate has good water solubility, and can effectively prevent the aggregation of the nano-silicon dioxide when the nano-silicon dioxide is prepared from the sodium silicate, thereby preparing the nano-silicon dioxide with large specific surface area, small particle size and narrow particle size distribution range.
The method for preparing the nano silicon dioxide by using the sodium silicate prepared by the technical scheme comprises the following preparation steps:
(1) preparing sodium silicate into a sodium silicate solution by using high-temperature steam;
(2) heating and stirring a part of sodium silicate solution, dropwise adding a sulfuric acid solution to adjust the pH value to 8-10, continuously heating and stirring, dropwise adding the rest of the sodium silicate solution and the sulfuric acid solution to keep the pH value at 8-10, continuously dropwise adding the sulfuric acid solution after the dropwise adding of the sodium silicate solution is finished until the pH value is 3-5, stopping dropwise adding the sulfuric acid solution, aging, press filtering, washing with water, spray drying, crushing, and calcining at high temperature under an oxygen atmosphere to obtain the nano-silica.
The mass concentration of the sodium silicate solution is 1-5%, and the concentration of the sulfuric acid solution is 1-5 mol/L.
The temperature of the high-temperature calcination is 300-400 ℃.
The specific surface area of the nano silicon dioxide is 300-500m2(iv)/g, average particle diameter of 5-50 nm.
The invention has the beneficial effects that: according to the invention, the refined quartz sand is used as the preparation raw material of the sodium silicate, so that the purification process of impurities is avoided, and the problem that the quality of the sodium silicate is influenced due to excessive impurities is solved; the invention also carries out surface modification on the sodium silicate, and utilizes the homemade cyclopropyl formamidine glutarate as a modifier, thereby improving the water solubility of the sodium silicate; meanwhile, the nano silicon dioxide further prepared by the prepared sodium silicate has the characteristics of small particle size and narrow particle size distribution range, so that the quality of the nano silicon dioxide is improved, and the application field of the nano silicon dioxide is widened.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Refined stoneThe Yingsha is prepared from Ganxin mineral product of Lingshu county, SiO2The content is 99-99.5%.
Example 1
Preparation of sodium silicate:
(1) 2kg of SiO2Mixing refined quartz sand with the content of more than 99% and 1kg of soda ash uniformly, sending the mixture into a horse shoe flame kiln, calcining the mixture at high temperature in the air atmosphere to perform a melting reaction, calcining the mixture at 1500 ℃ for 8 hours, quenching the mixture with water after the reaction is finished, and drying the mixture in a drying oven at 110 ℃ to obtain a crude sodium silicate product;
(2) crushing the crude sodium silicate into particles, then sending the particles into a high-pressure reaction kettle, introducing saturated water vapor at 150 ℃ for dissolving, filtering after complete dissolution, and taking filtrate to obtain a pure sodium silicate product;
(3) adding 0.05mol of glutaric acid and 0.1mol of (Z) -N-hydroxycyclopropanecarboxamidine into water, heating and stirring, then dropwise adding concentrated sulfuric acid, carrying out heat preservation reaction at 80 ℃ for 3 hours, adding ethyl acetate for extraction after the reaction is finished, taking an organic phase, concentrating to remove ethyl acetate, and carrying out column chromatography (a mixed solvent of ethyl acetate and petroleum ether is used as an eluent) to obtain cyclopropylformamidine glutarate;1H NMR(DMSO-d6,400MHz),:6.38(s,4H),2.28(t,4H),2.01(m,2H),0.15-0.34(m,10H)；ESI-MS:m/z＝298.15[M+2]+.
(4) adding 0.1kg of cyromazine glutarate into 1kg of sodium silicate pure product, mixing for 10min at the rotating speed of 1200r/min, concentrating to remove water, drying in a drying oven at 110 ℃, and crushing to obtain the sodium silicate with the modulus of 2.75-2.80.
Example 2
Example 2 differs from example 1 in that the amount of cyromazine glutarate was adjusted to 0.05 kg.
Preparation of sodium silicate:
(1) 2kg of SiO2Mixing refined quartz sand with the content of more than 99% and 1kg of soda ash uniformly, sending the mixture into a horse shoe flame kiln, calcining the mixture at high temperature in the air atmosphere to perform a melting reaction, calcining the mixture at 1500 ℃ for 8 hours, quenching the mixture with water after the reaction is finished, and drying the mixture in a drying oven at 110 ℃ to obtain a crude sodium silicate product;
(2) crushing the crude sodium silicate into particles, then sending the particles into a high-pressure reaction kettle, introducing saturated water vapor at 150 ℃ for dissolving, filtering after complete dissolution, and taking filtrate to obtain a pure sodium silicate product;
(3) adding 0.05mol of glutaric acid and 0.1mol of (Z) -N-hydroxycyclopropanecarboxamidine into water, heating and stirring, then dropwise adding concentrated sulfuric acid, carrying out heat preservation reaction at 80 ℃ for 3 hours, adding ethyl acetate for extraction after the reaction is finished, taking an organic phase, concentrating to remove ethyl acetate, and carrying out column chromatography (a mixed solvent of ethyl acetate and petroleum ether is used as an eluent) to obtain cyclopropylformamidine glutarate;1H NMR(DMSO-d6,400MHz),:6.38(s,4H),2.28(t,4H),2.01(m,2H),0.15-0.34(m,10H)；ESI-MS:m/z＝298.15[M+2]+.
(4) adding 0.05kg of cyromazine glutarate into 1kg of pure sodium silicate, mixing at the rotation speed of 1200r/min for 10min, concentrating to remove water, drying in a drying oven at 110 ℃, and crushing to obtain the sodium silicate with the modulus of 2.75-2.80.
Comparative example 1
Comparative example 1 differs from example 1 in that no cyclopropanecarboxamidine glutarate was prepared and added.
Preparation of sodium silicate:
(1) 2kg of SiO2Mixing refined quartz sand with the content of more than 99% and 1kg of soda ash uniformly, sending the mixture into a horse shoe flame kiln, calcining the mixture at high temperature in the air atmosphere to perform a melting reaction, calcining the mixture at 1500 ℃ for 8 hours, quenching the mixture with water after the reaction is finished, and drying the mixture in a drying oven at 110 ℃ to obtain a crude sodium silicate product;
(2) crushing the crude sodium silicate into particles, then sending the particles into a high-pressure reaction kettle, introducing saturated water vapor at 150 ℃ for dissolving, filtering after complete dissolution, and taking filtrate to obtain a pure sodium silicate product;
(3) concentrating the pure sodium silicate product, removing water, drying in a drying oven at 110 ℃, and crushing to obtain the sodium silicate with the modulus of 2.75-2.80.
Example 3
Preparing nano silicon dioxide:
(1) 100g of sodium silicate prepared in example 1 was prepared into a sodium silicate solution with a mass concentration of 2.5% by using saturated steam with a pressure of 0.1 MPa;
(2) heating sodium silicate solution with the volume of 1/2 to 85 ℃, stirring, dropwise adding sulfuric acid solution with the concentration of 2mol/L to adjust the pH to 9, continuously heating and stirring, dropwise adding the rest sodium silicate solution and the sulfuric acid solution to keep the pH at 9, continuously dropwise adding the sulfuric acid solution until the pH is 4 after the dropwise adding of the sodium silicate solution is finished, stopping dropwise adding the sulfuric acid solution, aging, press filtering, water washing, spray drying, crushing, calcining at high temperature under oxygen atmosphere, and calcining at 400 ℃ for 5 hours to obtain the nano-silica.
Example 4
Example 4 differs from example 3 in that the sodium silicate prepared in example 1 was replaced with the sodium silicate prepared in example 2.
Preparing nano silicon dioxide:
(1) 100g of the sodium silicate prepared in example 2 was prepared into a sodium silicate solution with a mass concentration of 2.5% by using saturated steam with a pressure of 0.1 MPa;
(2) heating sodium silicate solution with the volume of 1/2 to 85 ℃, stirring, dropwise adding sulfuric acid solution with the concentration of 2mol/L to adjust the pH to 9, continuously heating and stirring, dropwise adding the rest sodium silicate solution and the sulfuric acid solution to keep the pH at 9, continuously dropwise adding the sulfuric acid solution until the pH is 4 after the dropwise adding of the sodium silicate solution is finished, stopping dropwise adding the sulfuric acid solution, aging, press filtering, water washing, spray drying, crushing, calcining at high temperature under oxygen atmosphere, and calcining at 400 ℃ for 5 hours to obtain the nano-silica.
Comparative example 2
Comparative example 2 is different from example 3 in that the sodium silicate prepared in example 1 was replaced with the sodium silicate prepared in comparative example 1 and the conditions of high-temperature steam were modified, otherwise the sodium silicate could not be dissolved.
Preparing nano silicon dioxide:
(1) 100g of the sodium silicate prepared in comparative example 1 was prepared into a sodium silicate solution with a mass concentration of 2.5% by using saturated steam with a pressure of 0.3 MPa;
(2) heating sodium silicate solution with the volume of 1/2 to 85 ℃, stirring, dropwise adding sulfuric acid solution with the concentration of 2mol/L to adjust the pH to 9, continuously heating and stirring, dropwise adding the rest sodium silicate solution and the sulfuric acid solution to keep the pH at 9, continuously dropwise adding the sulfuric acid solution until the pH is 4 after the dropwise adding of the sodium silicate solution is finished, stopping dropwise adding the sulfuric acid solution, aging, press filtering, water washing, spray drying, crushing, calcining at high temperature under oxygen atmosphere, and calcining at 400 ℃ for 5 hours to obtain the nano-silica.
The physical parameters of the nano-silica prepared in the above examples and comparative examples are shown in table 1.
TABLE 1
| Item | Example 3 | Example 4 | Comparative example 2 |
| Specific surface area, m2/g | 420 | 350 | 180 |
| Average particle diameter, nm | 15-25 | 20-50 | 300-400 |
As can be seen from Table 1, the surface modification of sodium silicate by the cyprocoamidine glutarate can improve the specific surface area of the nano-silica prepared from the sodium silicate, and the nano-silica with small particle size and narrow particle size distribution range is successfully prepared.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. A method for preparing sodium silicate for nano silicon dioxide is characterized by comprising the following steps: the preparation method comprises the following preparation steps:
(1) mixing Si02Mixing refined quartz sand with the content of more than 99% and soda ash uniformly, then sending the mixture into a horse shoe flame kiln, calcining the mixture at high temperature in air atmosphere to perform melting reaction, quenching the mixture with water after the reaction is finished, and drying the mixture to obtain a sodium silicate crude product;
(2) crushing the crude sodium silicate into particles, then sending the particles into a high-pressure reaction kettle, introducing high-temperature steam for dissolving, filtering after complete dissolution, and taking filtrate to obtain a pure sodium silicate product;
(3) adding glutaric acid and (Z) -N-hydroxycyclopropanecarboxamidine into water, heating and stirring, then dropwise adding concentrated sulfuric acid, keeping the temperature for reaction, adding ethyl acetate for extraction after the reaction is finished, taking an organic phase, concentrating to remove ethyl acetate, and carrying out column chromatography to obtain cyclopropanecarboxamidine glutarate;
(4) adding the methyl cyclopropaneamidine glutarate into the pure sodium silicate, mixing at high speed, concentrating to remove water, drying and crushing to obtain the sodium silicate.
2. The method for preparing sodium silicate for nano-silica according to claim 1, characterized in that: the mass ratio of the refined quartz sand to the soda ash is 2-3: 1.
3. The method for preparing sodium silicate for nano-silica according to claim 1, characterized in that: the temperature of the melting reaction was 1450-.
4. The method for preparing sodium silicate for nano-silica according to claim 1, characterized in that: the temperature of the high-temperature steam is 145-160 ℃, and the pressure is 0.4-0.6 MPa.
5. The method for preparing sodium silicate for nano-silica according to claim 1, characterized in that: the mole ratio of glutaric acid to (Z) -N-hydroxycyclopropanecarboxamidine is 1: 2-2.05.
6. The method for preparing sodium silicate for nano-silica according to claim 1, characterized in that: the temperature of the heat preservation reaction is 70-90 ℃.
7. The method for preparing sodium silicate for nano-silica according to claim 1, characterized in that: the mass ratio of the pure sodium silicate to the cyclopropyl formamidine glutarate is 1: 0.05-0.2.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003070636A1 (en) * | 2001-12-21 | 2003-08-28 | Tianrun Ye | Method of producing a silica aerogel and a sodium carbonate |
| US20080199385A1 (en) * | 2005-06-08 | 2008-08-21 | Evonik Degussa Wellink Silica(Nanping) Co. Ltd. | Process for Producing Silica and Sodium Sulfite with Sodium Sulfate |
| US20080202387A1 (en) * | 2005-06-08 | 2008-08-28 | Yuanjian Lu | Process For Producing Silica and Sodium Sulfite With Sodium Sulfate |
| CN103466637A (en) * | 2013-08-29 | 2013-12-25 | 中国科学院过程工程研究所 | Method for producing precipitate silicon dioxide by using sodium bicarbonate to control supersaturation degree |
| CN109264731A (en) * | 2018-09-19 | 2019-01-25 | 安徽龙泉硅材料有限公司 | The ultrapure sodium metasilicate of high-temperature silicon disulfide rubber reinforcing agent |
| CN110040738A (en) * | 2019-05-05 | 2019-07-23 | 安徽龙泉硅材料有限公司 | A kind of production method for processing green tire reinforcing agent sodium metasilicate |
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2020
- 2020-06-22 CN CN202010573736.3A patent/CN111620348B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003070636A1 (en) * | 2001-12-21 | 2003-08-28 | Tianrun Ye | Method of producing a silica aerogel and a sodium carbonate |
| US20080199385A1 (en) * | 2005-06-08 | 2008-08-21 | Evonik Degussa Wellink Silica(Nanping) Co. Ltd. | Process for Producing Silica and Sodium Sulfite with Sodium Sulfate |
| US20080202387A1 (en) * | 2005-06-08 | 2008-08-28 | Yuanjian Lu | Process For Producing Silica and Sodium Sulfite With Sodium Sulfate |
| CN103466637A (en) * | 2013-08-29 | 2013-12-25 | 中国科学院过程工程研究所 | Method for producing precipitate silicon dioxide by using sodium bicarbonate to control supersaturation degree |
| CN109264731A (en) * | 2018-09-19 | 2019-01-25 | 安徽龙泉硅材料有限公司 | The ultrapure sodium metasilicate of high-temperature silicon disulfide rubber reinforcing agent |
| CN110040738A (en) * | 2019-05-05 | 2019-07-23 | 安徽龙泉硅材料有限公司 | A kind of production method for processing green tire reinforcing agent sodium metasilicate |
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