CN107162009B - Preparation method of high-structure high-wear-resistance hydrated silicon dioxide - Google Patents
Preparation method of high-structure high-wear-resistance hydrated silicon dioxide Download PDFInfo
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- CN107162009B CN107162009B CN201710451487.9A CN201710451487A CN107162009B CN 107162009 B CN107162009 B CN 107162009B CN 201710451487 A CN201710451487 A CN 201710451487A CN 107162009 B CN107162009 B CN 107162009B
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- sodium silicate
- silicon dioxide
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- hydrated silicon
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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
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- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of high-structure high-wear-resistance hydrated silicon dioxide, which is characterized by comprising the following steps: (1) calcining quartz sand and sodium carbonate at the temperature of 1420-1450 ℃ for 1 hour according to the molar ratio of 1:1.5 to obtain solid sodium silicate; (2) dissolving solid sodium silicate in sodium carbonate to obtain a sodium silicate solution, and filtering to remove impurities; (3) adding a dispersing agent into the sodium silicate solution, and dropwise adding 4-6mol/L sulfuric acid solution into the sodium silicate solution under the stirring condition to separate out a precipitate; 4) washing and drying the precipitate to obtain the hydrated silicon dioxide. By the preparation method, the high-structure and high-wear-resistance hydrated silicon dioxide can be prepared.
Description
Technical Field
The invention relates to the field of organic matter preparation, in particular to a preparation method of high-structure high-wear-resistance hydrated silicon dioxide.
Background
Hydrated silica, also known as light silica, has the main components of silica, white amorphous powder, light and loose, soluble in caustic alkali and hydrofluoric acid, and insoluble in water, solvents and acids (except hydrofluoric acid). High-temperature resistance, non-combustion, tastelessness, odorless and good electrical insulation. It behaves similarly to carbon black, but is white. SiO with molecular formula and structural formula2·nH2O represents, wherein nH2O is present in the form of surface hydroxyl groups. The macro structure is similar to carbon black, the particles are spherical, and the single particles are in surface contact with each other and form a chain-shaped connection structure (secondary structure). The chain branch structure acts with hydrogen bond force to form a cluster aggregate. The surface of the hydrated silicon dioxide particle has hydroxyl, and mainly comprises three types of isolated hydroxyl, adjacent hydroxyl and siloxy. The adjacent hydroxyl groups are very important for the adsorption of polar substances, the surface of the material has strong hydrophilicity due to the existence of the groups, the surface area and the dispersing capacity are large, and the mechanical strength and the tearing resistance index are high. High insulation, small particles, large specific surface area, high structure and the like. However, in the current production, it is difficult to achieve high structure of hydrated silica.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of high-structure high-wear-resistance hydrated silicon dioxide.
Namely, the invention provides a preparation method of high-structure high-wear-resistance hydrated silica, which comprises the following steps:
(1) calcining quartz sand and sodium carbonate at the temperature of 1420-1450 ℃ for 1 hour according to the molar ratio of 1:1.2-1.4 to obtain solid sodium silicate;
(2) dissolving solid sodium silicate in 3-5mol/L sodium carbonate to obtain sodium silicate solution, and filtering to remove impurities;
(3) adding a dispersing agent into the sodium silicate solution, and dropwise adding 4-6mol/L sulfuric acid solution into the sodium silicate solution under the stirring condition to separate out a precipitate;
(4) washing and drying the precipitate to obtain the hydrated silicon dioxide.
Wherein the dispersant is sodium lignosulfonate.
In addition, the molar ratio of the sodium silicate to the sodium carbonate to the dispersant to the sulfuric acid is 1: 1.2-1.5:0.2-0.5: 1.2-1.5.
Further, the dropping speed of the sulfuric acid solution was 5mol/h in terms of sulfuric acid.
Sodium lignosulfonate is a natural high-molecular polymer, an anionic surfactant, has strong dispersing capacity and is suitable for dispersing solids in an aqueous medium. The polymer has different dispersivity due to different molecular weight and functional groups, can be adsorbed on the surface of various solid particles, can perform metal ion exchange, and can generate condensation or hydrogen bond with other compounds due to the existence of various active groups on the organization structure. Sodium lignosulfonates are widely used in industry as dispersing and wetting agents.
According to the invention, sodium lignosulfonate is used as a dispersing agent, and the dropping speed of sulfuric acid is controlled, so that high-structure hydrated silicon dioxide can be prepared, and the hydrated silicon dioxide is found to have high wear resistance.
Detailed Description
The present invention will be described in detail with reference to the following examples, but the present invention is not limited to the examples, and alternatives to the conventional techniques fall within the scope of the present invention.
Example 1
(1) Calcining 5mol of quartz sand and 6mol of soda ash at 1420 ℃ for 1 hour to obtain solid sodium silicate;
(2) dissolving 4.5mol of solid sodium silicate in 1.8L of sodium carbonate with the concentration of 3mol/L to obtain a sodium silicate solution, and filtering to remove impurities;
(3) adding 0.9mol of dispersant into the sodium silicate solution, and dripping 6mol/L of sulfuric acid solution into the sodium silicate solution under the stirring condition to obtain 1.125L, wherein the dripping speed is 5mol/L, and precipitates are separated out;
(4) washing and drying the precipitate to obtain the hydrated silicon dioxide.
Example 2
(1) Calcining 5mol of quartz sand and 7mol of soda ash at 1450 ℃ for 1 hour to obtain solid sodium silicate;
(2) dissolving 4.5mol of solid sodium silicate in 1.35L of sodium carbonate with the concentration of 5mol/L to obtain a sodium silicate solution, and filtering to remove impurities;
(3) adding 2.25mol of dispersant into the sodium silicate solution, and dripping 4mol/L of sulfuric acid solution into the sodium silicate solution under the stirring condition for 1.35L at the dripping speed of 5mol/h to separate out a precipitate;
(4) washing and drying the precipitate to obtain the hydrated silicon dioxide.
Example 3
(1) Calcining 5mol of quartz sand and 6.5mol of soda ash at 1450 ℃ for 1 hour to obtain solid sodium silicate;
(2) dissolving 4.5mol of solid sodium silicate in 1.575L of sodium carbonate with the concentration of 4mol/L to obtain a sodium silicate solution, and filtering to remove impurities;
(3) 1.35mol of dispersant is added into the sodium silicate solution, 1.26L of 5mol/L sulfuric acid solution is dripped into the sodium silicate solution under the condition of stirring, the dripping speed is 5mol/h, and precipitates are separated out;
(4) washing and drying the precipitate to obtain the hydrated silicon dioxide.
The hydrated silica obtained in examples 1 to 3 was subjected to structural analysis, and the proportion of the ortho-hydroxyl groups on silicon was 70 to 90%, which was referred to as a high-structure hydrated silica.
The rubber processing was carried out according to HG/T2404-2008 "identification of hydrated silica in styrene-butadiene rubber". Shore hardness was measured according to GB/T531 and tear strength was measured according to GB/T529. Commercially available hydrated silicas are comparative examples. The hydrated silica of examples 1 to 3 and comparative example was used as a filler, and compounded with styrene-butadiene rubber, an accelerator, a coupling agent and the like to prepare a tread rubber for a tire, followed by vulcanization molding at a high temperature. The Treadwear index was determined and the results are shown in the table below.
TABLE 1
As can be seen from Table 1, the hydrated silica prepared by the present invention has high abrasion resistance in combination with a high structure.
Claims (2)
1. A preparation method of high-structure high-wear-resistance hydrated silica is characterized by comprising the following steps:
(1) calcining quartz sand and sodium carbonate at the temperature of 1420-1450 ℃ for 1 hour according to the molar ratio of 1:1.2-1.4 to obtain solid sodium silicate;
(2) dissolving solid sodium silicate in 3-5mol/L sodium carbonate to obtain sodium silicate solution, and filtering to remove impurities;
(3) adding a dispersing agent into the sodium silicate solution, and dropwise adding 4-6mol/L sulfuric acid solution into the sodium silicate solution under the stirring condition to separate out a precipitate;
(4) washing and drying the precipitate to obtain hydrated silicon dioxide;
in the step (3), the dropping speed of the sulfuric acid solution is 5mol/h calculated by sulfuric acid;
the dispersant is sodium lignosulfonate.
2. The preparation method according to claim 1, wherein the molar ratio of the sodium silicate, the sodium carbonate, the dispersant and the sulfuric acid is 1: 1.2-1.5:0.2-0.5: 1.2-1.5.
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| CN109205632A (en) * | 2018-09-19 | 2019-01-15 | 安徽龙泉硅材料有限公司 | The ultrapure sodium metasilicate of delustering agent |
| CN114516637A (en) * | 2022-03-24 | 2022-05-20 | 福建省三明同晟化工有限公司 | High additive feed additive silicon dioxide and preparation method thereof |
| CN114804121A (en) * | 2022-03-24 | 2022-07-29 | 福建省三明同晟化工有限公司 | Preparation method of silica for glass cement for shoes |
| CN114560471A (en) * | 2022-03-25 | 2022-05-31 | 福建省三明同晟化工有限公司 | Silica for wear-resistant tire rubber and preparation method thereof |
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| US3219590A (en) * | 1961-08-01 | 1965-11-23 | Union Carbide Corp | Bonded molecular sieves |
| CN101172608B (en) * | 2006-10-31 | 2010-10-06 | 中南大学 | Method of producing high-specific area nano-silicon dioxide |
| CN103466637B (en) * | 2013-08-29 | 2015-06-03 | 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 |
| CN103754885B (en) * | 2014-01-26 | 2015-09-02 | 乌鲁木齐金石徽龙矿业有限公司 | The method of porous silica is prepared in a kind of acidleach |
| CN106276929B (en) * | 2016-07-29 | 2017-07-07 | 广州市飞雪材料科技有限公司 | A kind of preparation method of friction type silica |
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