CN1482061A - Method for producing nanometer silicon dioxide using datolite - Google Patents
Method for producing nanometer silicon dioxide using datolite Download PDFInfo
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Abstract
The process of producing nano SiO2 with wollastonite as material includes the steps of: adding dispersant, wollastonite powder and hydrochloric acid into chemical reactor with hot water to produce chemical reaction; regulating the pH value of the reacted liquid mixture first with alkali liquid to 4-7 and then with hydrochloric acid to lower than 2; filtering out and tumble-drying the product and transferring the product into one other chemical reactor with hot water; adding hydrochloric acid for secondary reaction; filtering the product silica gel after finishing the reaction; and washing, tumble-drying, soaking in alcohol, tert-butyl alcohol or n-butyl alcohol for protection, stoving and igniting to obtain the product. The present invention features the direct production process from ore to nano SiO2, and has the advantages of simple technological process, short flow path, low power consumption, stable quality and low production cost.
Description
The invention relates to a method for producing non-metallic nano materials, in particular to a method for producing nano silicon dioxide by using wollastonite as a raw material.
The nano silicon dioxide as an additive can be widely applied to the fields of plastics, rubber, ceramics, sealants, adhesives, glass fiber reinforced plastics, pigments, coatings, functional fibers, organic glass, environmental protection adsorption, printing and dyeing, papermaking and the like, and the performance of the original product is greatly improved after the nano silicon dioxide is used. The existing production methods of nano silicon dioxide have three types: sodium silicate (water glass), silica sol and tetraethoxysilane. The common characteristics of the production methods are large investment of fixed assets, complex process, large water consumption, high energy consumption and high production cost.
The invention aims to provide a method for producing nano silicon dioxide by using wollastonite as a raw material, which has the advantages of small investment, simple process and low cost.
The technical scheme of the invention is to produce the nano-scale silicon dioxide by using wollastonite with low price and rich resources as a raw material, applying a sol-gel process, protecting by a dispersing agent and controlling the pH value of a reaction system. The wollastonite has the chemical name of calcium metasilicate and the molecular formula: CaSiO3. The molecular formula of the product silicon dioxide is SiO2. Adding 0.1-1.5 wt% of dispersant polyethylene glycol into a chemical reactor filled with hot water, starting a stirrer, stirring uniformly, adding wollastonite powder to prepare 5-15 wt% of water suspension, adding hydrochloric acid to react, adding 0.05-0.50 wt% of hydrofluoric acid during the reaction, controlling the pH value of the reaction system to be always less than 2 according to the speed and the adding amount of hydrochloric acid, neutralizing with alkaline solution after the reaction is finished, adjusting the pH value of the mixed solution to 4-7, adjusting the pH value of the mixed solution to be less than 2 with hydrochloric acid, filtering, washing and drying a product silica gel (precipitated hydrated silicon dioxide), adding the product silica gel into the chemical reactor filled with hot water and containing 0.1-1.0 wt% of polyethylene glycol, adding hydrochloric acid to carry out a secondary reaction, controlling the pH value of the reaction system to be always less than 2, filtering, washing and drying the product silica gel after the reaction is finished, and using alcohol, Immersing tert-butyl alcohol or n-butyl alcohol for protection, drying in a dryer, burning in a burning furnace at 600-750 deg.C to remove polyethylene glycol as dispersant, and getting final product.
The reaction mechanism of the target product is as follows:
the product quality is as follows: SiO 22≥98.5％；MgO≤0.2％；CaO≤0.5％；Fe2O3Less than or equal to 0.1 percent; other impurities are less than or equal to 0.7 percent; the particle diameter is 5-100 nanometers, and the specific surface area is more than or equal to 250m2(ii)/g; the whiteness is more than or equal to 91.
Compared with the prior art, the invention has the advantages that:
1. the method for preparing the nano material from the wollastonite by using the ore in one step has the advantages of simple process, short flow, low energy consumption, low production cost and low water consumption which is only half of that of a sodium silicate method.
2. The industrial production equipment is general chemical equipment, is used for a small amount of professional production equipment, has low investment on fixed assets and is only 50 percent of the investment of a sodium silicate method of the same specification.
3. Alcohol, tertiary butanol or n-butanol are used for protecting the produced nano-scale silicon dioxide, so that the growth of silicon dioxide particles can be effectively prevented, and the particle size is controlled within 100 nanometers.
The present invention will be described in further detail with reference to examples.
Example (b):
the invention adopts the technical scheme that the sol-gel process and the dispersant are used for protection, and the PH value of a reaction system is controlled to produce the nano silicon dioxide, and the specific implementation is as follows: adding 0.1-1.5 wt% of dispersant polyethylene glycol into a chemical reactor containing hot water, starting a stirrer, stirring to uniformly distribute polyethylene glycol in the hot water, adding wollastonite powder to prepare 5-15 wt% of water suspension, adding hydrochloric acid to carry out chemical reaction, adding 0.05-0.50 wt% of hydrofluoric acid during the reaction, controlling the pH value of the reaction system to be always less than 2 according to the speed and the adding amount of hydrochloric acid, neutralizing with alkaline solution after the reaction is finished, adjusting the pH value of the mixed solution to 4-7, adjusting the pH value of the mixed solution to be less than 2 with hydrochloric acid, filtering, washing and drying the product silica gel (precipitated hydrated silica), adding the product into another chemical reactor containing 0.1-1.0 wt% of polyethylene glycol in hot water, adding hydrochloric acid to carry out secondary reaction, controlling the pH value of the reaction system to be always less than 2, and after the reaction is finished, filtering the product silica gel, cleaning, spin-drying, immersing and protecting the product silica gel with alcohol, tert-butyl alcohol or n-butyl alcohol, pouring the product silica gel into a dryer for drying, then putting the product silica gel into an ignition furnace, and igniting the product silica gel at the temperature of 600-750 ℃ to remove the dispersant polyethylene glycol, thus obtaining the finished product of the nano silicon dioxide.
Example 1: weighing 10 percent of wollastonite powder produced in the new Jiangxi province, accounting for 100 kg, and 1.0 percent of polyethylene glycol dispersant, accounting for 10 kg for standby. Adding hot water of 40-60 ℃ into a chemical reactor, accounting for 888 kg of hot water accounting for 88.8 percent, adding polyethylene glycol, starting a stirrer, stirring uniformly, adding wollastonite powder to prepare 10 percent aqueous suspension, adding hydrochloric acid to carry out chemical reaction, adding 0.20 percent of hydrofluoric acid accounting for 2.0 kg of hydrofluoric acid during the reaction, removing impurities such as magnesium, iron, aluminum, manganese and the like, controlling the pH value of a reaction system to be always less than 2 according to the speed and the adding amount of hydrochloric acid during the reaction, and frequently measuring by using pH test paper or an acidimeter. And after the reaction is finished, neutralizing and adjusting the pH value of the mixed solution after the reaction to 4-5 by using ammonia water, adjusting the pH value of the mixed solution back to be less than 2 by using hydrochloric acid, filtering, washing and spin-drying the product silica gel, putting the product silicagel into another chemical reactor filled with hot water and containing 0.8% of polyethylene glycol, adding hydrochloric acid, carrying out secondary reaction, and further removing impurities such as calcium, magnesium, iron, manganese, aluminum and the like. In the reaction process, the acid adding speed and the adding amount are subject to the control that the pH value of the reaction system is always less than 2. After the reaction is finished, filtering, cleaning and drying the product silica gel, immersing the product silica gel in alcohol for protection, pouring the product silica gel into a dryer for drying, taking out the product silica gel, putting the product silica gel into a firing furnace, and firing the product at the temperature of 600-750 ℃ to remove the dispersant polyethylene glycol to obtain a finished product.
Example 2:
weighing 5 percent of the Jiangxi high-yield wollastonite powder and 50 kg of the dispersant polyethylene glycol, and 0.1 percent of the dispersant polyethylene glycol and 1 kg of the dispersant polyethylene glycol for standby. Adding 94.85% of clean water into a chemical reactor, accounting for 948.5 kg, heating to 50-60 ℃ by using a heater, adding polyethylene glycol, starting a stirrer, adding wollastonite powder after uniformly stirring to prepare 5% of water suspension, adding hydrochloric acid to perform chemical reaction, adding 0.05% of 0.5 kg of hydrofluoric acid during the reaction, controlling the pH value of a reaction system to be always less than 2, neutralizing and adjusting the pH value of the reacted mixed solution to 5-7 by using a sodium hydroxide solution after the reaction is finished, adjusting the pH value of the mixed solution to be less than 2 by using hydrochloric acid, filtering, washing and spin-drying the product silica gel for later use. Discharging and cleaning the residual liquid in the chemical reactor, adding clean water again, heating to 70-80 ℃, adding 0.1% of polyethylene glycol, stirring uniformly, adding the product silica gel of the previous reaction, adding hydrochloric acid, carrying out a secondary reaction, and controlling the pH value of the reaction system to be less than 2 all the time. After the reaction is finished, filtering, cleaning and drying the product, immersing and protecting the product by using tert-butyl alcohol, and drying and firing the product to obtain the product.
Example 3:
weighing 15 percent of the Jiangxi high-yield wollastonite powder, counting 300 kg, and 1.5 percent of polyethylene glycol, counting 30 kg for standby. Injecting 70-90 ℃ hot water into a chemical reactor, measuring 1660 kg, adding polyethylene glycol, starting a stirrer, uniformly stirring, adding wollastonite powder to prepare 15% aqueous suspension, adding hydrochloric acid to carry out chemical reaction, adding 0.50% 10 kg of hydrofluoric acid during the reaction, controlling the pH value of a reaction system to be always less than 2, neutralizing and adjusting the pH value of the mixed solution after the reaction to 4-7 by using a calcium hydroxide solution after the reaction is finished, adjusting the pH value of the mixed solution to be less than 2 by using hydrochloric acid, filtering, washing and drying the product silica gel, placing the product into another reactor which contains 1.0% of polyethylene glycol and contains hot water, adding hydrochloric acid to carry out secondary reaction, and controlling the pH value of the reaction system to be always less than 2. After the reaction is finished, filtering, cleaning and drying the product, immersing the product in butanol for protection, and drying and firing the product to obtain the product.
Claims (1)
1. A method for producing nano silicon dioxide by using wollastonite as a raw material sequentially comprises thefollowing steps:
(1) adding 0.1 to 1.5 percent of dispersant polyethylene glycol into a chemical reactor filled with hot water;
(2) after being stirred evenly, wollastonite powder is added to prepare 5 to 15 percent of water suspension;
(3) adding hydrochloric acid, and controlling the pH value of the reaction system to be less than 2 all the time;
(4) 0.05 to 0.50 percent of hydrofluoric acid is added during the reaction period;
(5) neutralizing with alkali liquor to adjust the pH value of the mixed liquor after reaction to 4-7;
(6) adjusting the pH value of the mixed solution to be less than 2 by hydrochloric acid;
(7) filtering, washing and drying the product, and putting the product into a chemical reactor which contains hot water and 0.1 to 1.0 percent of polyethylene glycol;
(8) adding hydrochloric acid, and controlling the pH value of the reaction system to be less than 2 all the time;
(9) filtering, cleaning and drying the product, and immersing and protecting the product by using alcohol, tert-butyl alcohol or n-butyl alcohol;
(10) putting the product into a dryer for drying;
(11) taking out and putting into a burning furnace, burning at the temperature of 600-750 ℃, and removing the polyethylene glycol serving as the dispersant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 02143002 CN1274592C (en) | 2002-09-10 | 2002-09-10 | Method for producing nanometer silicon dioxide using datolite |
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| CN 02143002 CN1274592C (en) | 2002-09-10 | 2002-09-10 | Method for producing nanometer silicon dioxide using datolite |
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| CN1482061A true CN1482061A (en) | 2004-03-17 |
| CN1274592C CN1274592C (en) | 2006-09-13 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428805B (en) * | 2008-12-03 | 2011-06-29 | 湖北永绍科技有限公司 | Utilization technology for fluorine-containing white residue |
| CN103213992A (en) * | 2013-04-15 | 2013-07-24 | 沈阳理工大学 | Method for preparing nano white carbon black by taking wollastonite as raw material |
| CN104004385A (en) * | 2014-05-13 | 2014-08-27 | 天津科技大学 | Preparation method of modified wollastonite used as papermaking filling materials |
| CN106145128A (en) * | 2016-08-18 | 2016-11-23 | 柳州市亿廷贸易有限责任公司 | The method preparing nano silicon for raw material with wollastonite |
| CN113562738A (en) * | 2021-08-17 | 2021-10-29 | 西安理工大学 | Method for purifying silicon dioxide by using micro silicon powder |
-
2002
- 2002-09-10 CN CN 02143002 patent/CN1274592C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428805B (en) * | 2008-12-03 | 2011-06-29 | 湖北永绍科技有限公司 | Utilization technology for fluorine-containing white residue |
| CN103213992A (en) * | 2013-04-15 | 2013-07-24 | 沈阳理工大学 | Method for preparing nano white carbon black by taking wollastonite as raw material |
| CN103213992B (en) * | 2013-04-15 | 2014-12-10 | 沈阳理工大学 | Method for preparing nano white carbon black by taking wollastonite as raw material |
| CN104004385A (en) * | 2014-05-13 | 2014-08-27 | 天津科技大学 | Preparation method of modified wollastonite used as papermaking filling materials |
| CN104004385B (en) * | 2014-05-13 | 2016-01-20 | 天津科技大学 | A kind of preparation method of the modified grammite for papermaking filler |
| CN106145128A (en) * | 2016-08-18 | 2016-11-23 | 柳州市亿廷贸易有限责任公司 | The method preparing nano silicon for raw material with wollastonite |
| CN113562738A (en) * | 2021-08-17 | 2021-10-29 | 西安理工大学 | Method for purifying silicon dioxide by using micro silicon powder |
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| Publication number | Publication date |
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| CN1274592C (en) | 2006-09-13 |
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