CN110844911A - Method for directly preparing high-purity white carbon black by using fluorine-containing silicon slag - Google Patents
Method for directly preparing high-purity white carbon black by using fluorine-containing silicon slag Download PDFInfo
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- CN110844911A CN110844911A CN201911321893.9A CN201911321893A CN110844911A CN 110844911 A CN110844911 A CN 110844911A CN 201911321893 A CN201911321893 A CN 201911321893A CN 110844911 A CN110844911 A CN 110844911A
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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
- C01B33/186—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof from or via fluosilicic acid or salts thereof by a wet process
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/50—Fluorides
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- 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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- 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
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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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention relates to a method for directly preparing high-purity white carbon black by utilizing fluorine-containing silicon slag, which comprises the steps of homogenizing, pulping and dispersing the fluorine-containing silicon slag, so that aluminum hydroxide powder wrapped in solid white carbon black particles is dispersed to react with fluosilicic acid adsorbed by the solid white carbon black, and an aluminum fluoride solution and a solid silicon dioxide material which are dissolved in water are generated; removing acid liquor containing aluminum fluoride, and carrying out at least one time of homogenizing pulping, dispersing and ultrasonic fine washing on the obtained solid silicon dioxide material until washing water is neutral; and dehydrating and drying the neutral silicon dioxide material to obtain the high-quality white carbon black. The method is simple and practical, can be used for industrial production, and the prepared SiO in the white carbon black2Content (dry basis) is not less than 92%, NSA is not less than 200g/m2The particle size is less than or equal to 0.044um, and the total iron content is less than or equal to 0.01 percent; other technical indexes all meet or exceed the requirements of national industrial standard HG/T3061-2009 of precipitated white carbon black.
Description
Technical Field
The invention relates to a method for directly preparing high-purity white carbon black by using fluorine-containing silicon slag, belonging to the technical field of solid waste mineral deep processing and environmental protection.
Background
The existing process route for producing aluminum fluoride by using the byproduct fluosilicic acid is as follows: fluosilicic acid and aluminum hydroxide are used as raw materials, reaction is carried out at the temperature of 80-100 ℃, and a vacuum belt filter is used for separating water-soluble aluminum fluoride and generating solid white carbon black. The white carbon black particles are porous, spherical in surface, many in surface hydroxyl groups and extremely strong in chemical adsorption. The conventional chemical reaction kettle is adopted for preparing the aluminum fluoride by using the fluosilicic acid, the stirring rotating speed is low, the shearing force is small, and the white carbon black generated in the synthesis process is easy to adsorb with hydrogenated aluminum powder, fluosilicic acid and the like to form a mass so that the particle size is larger. The aluminum hydroxide powder and the white carbon black can not react with the fluosilicic acid after being wrapped together, so that the production cost is high. Therefore, the separated white carbon black has the characteristics of one large white carbon black, one small white carbon black, one low white carbon black and one high white carbon black: namely large particle size, small specific surface area, low purity (silicon dioxide content is 40-60%) and high fluorine content, and is generally called fluorine-containing silica slag. In the process of producing aluminum fluoride by using the actual fluosilicic acid, the silicon content in the silicon slag is measured to be 40-60% after the silicon slag is dried, and the aluminum content is measured to be 20-30%; and the two substances can not be separated, the two substances are often treated as garbage, and the fluorine ions can seriously pollute the surrounding environment. With the production of the slag in the year, the amount of the white carbon black (fluorine-containing silicon slag) produced as a byproduct is increased, and if the fluorine-containing silicon slag is not treated timely and effectively, the survival and the development of enterprises are restricted. Consulting the Chinese patent literature: authorization notice number: CN101428805B, using industrial hydrochloric acid containing HCl 30% as leaching solution to make Al in fluorine-containing silicon slag3+Formation of AlCl3While dissolving in an aqueous solution, F-And the fluosilicic acid is also dissolved out in sequence, and the main reaction formula is as follows: al (OH)3+3HCl→AlCl3+3H 2O; and (3) carrying out solid-liquid separation on the leaching solution and the silicon dioxide precipitate, repeatedly rinsing the separated solid silicon dioxide by deionized water according to the proportion, filtering to remove water, obtaining high-purity silicon dioxide, and further producing the water glass or white carbon black product. Chinese patent CN 101913637A, silica residue reacts with alkali liquor to prepare water glass, and then reacts with sulfuric acid to prepare the silicon glassWhite carbon black product. Chinese patent CN 103663474B, reacting fluorine-containing silicon slag with alkali liquor to obtain silicon dioxide and fluoride salt, then filtering and separating to obtain solid silicon dioxide and fluoride salt solution, and then washing the silicon dioxide. And drying to obtain the white carbon black product. In chinese patent CN 105036144B, acidic silica residue and sodium hydroxide are subjected to microwave reaction, solid-liquid separation is performed to obtain solid 1 and solution 1, then surfactant is added into the liquid 1 to obtain liquid 2, and the acid solution and the liquid 2 are mixed, aged, solid-liquid separated and dried to obtain the highly dispersed white carbon black product. The Chinese patent application publication No. CN 110156030A, the fluorine-containing silicon slag is put into a calcining kiln to be heated at 800 ℃ and 1700 ℃, the heat preservation is carried out for 1 to 10 hours, and then the low-fluorine and low-water white carbon black product with the granularity not more than 9um is prepared by cooling and crushing. The processes for preparing the white carbon black in the patents are complex, large in investment and difficult to realize industrialization, and the quality of the product cannot meet the requirements of national industry standards. Therefore, how to scientifically treat the silicon slag with large particle size, low purity, small specific surface area and high fluorine content to prepare the white carbon black product with high quality and exceeding the national industry standard requirement, and changing waste into valuable is the most urgent problem to be solved by enterprises.
Disclosure of Invention
The invention provides a simple, practical and industrialized method for directly preparing high-purity white carbon black by using fluorine-containing silicon slag, so that SiO in the prepared white carbon black2Content (dry basis) is not less than 92%, NSA: ≧ 200g/m2The particle size is less than or equal to 0.044um, and the total iron content is less than or equal to 0.01 percent; other technical indexes all meet or exceed the requirements of national industrial standard HG/T3061-2009 of precipitated white carbon black.
The invention solves the technical problems and adopts the scheme that:
a method for directly preparing high-purity white carbon black by utilizing fluorine-containing silicon slag comprises the following steps:
(1) firstly, carrying out homogenizing pulping and dispersing on fluorine-containing silicon slag to form stable suspension, so that aluminum hydroxide powder coated by white carbon black and fluosilicic acid adsorbed by the white carbon black can fully react to generate white carbon black and water-soluble aluminum fluoride;
(2) removing acid liquor containing aluminum fluoride, and carrying out at least one time of homogenizing pulping, dispersing and ultrasonic fine washing on the obtained solid silicon dioxide material until washing water is neutral, so that impurities in micropores of the white carbon black and impurities adsorbed on the surface of the white carbon black are separated to the maximum extent;
(3) and dehydrating and drying the neutral silicon dioxide material to obtain the high-quality white carbon black.
Preferably, before the fluorine-containing silicon slag is homogenized, pulped and dispersed in the step (1), deacidification treatment can be carried out on the fluorine-containing silicon slag.
Preferably, the step (2) adopts a centrifuge to perform plate and frame filter pressing and a centrifuge to perform combined deacidification treatment.
Preferably, the pulping treatment is carried out using a homogenizing kettle.
Preferably, tap water or pure water is adopted for pulping, the concentration of the slurry is controlled to be 10-30%, the pulping time is 1-6 hours, more preferably 3-5 hours, and particularly, the stable suspension formed by the slurry is taken as the standard.
Preferably, in the ultrasonic fine cleaning process, tap water or pure water is adopted to prepare the material into slurry with the concentration of 10-30%, the temperature is 45-65 ℃, and the ultrasonic treatment time is 60-100 min, more preferably 30-45 min.
Preferably, after the neutral silicon dioxide material obtained in the step (3) is dehydrated, homogenizing and pulping are carried out again before drying.
Preferably, the dehydrated silica material is spray or flash dried.
Compared with the prior art, the invention has the following advantages:
1, the process is short and practical; 2, the investment is low and the effect is quick; 3, the production cost is low; 4, the required field is small; 5, the product has high purity and large specific surface area.
2, the invention uses a homogenizing beater to carry out beating dispersion on the white carbon black to form stable suspension: aluminum hydroxide powder originally wrapped in the white carbon black is dispersed and then fully reacts with fluosilicic acid adsorbed by the white carbon black to generate water-soluble aluminum fluoride and water-insoluble white carbon black, and a part of aluminum fluoride can be recycled, so that the yield of reactants for producing aluminum fluoride from fluosilicic acid is improved.
3, because the generated white carbon black has the characteristics of fine particle size, more pore channels in the particles, large specific surface area, large surface energy, strong adsorbability and the like, under the action of strong bubble impact force provided by ultrasonic waves, fine particle impurities, acid liquor and impurity particles adsorbed by the surface of the white carbon black in the original white carbon black micropore channels are all cleaned out, so that the purity of the white carbon black can be improved.
4, homogenizing, pulping and dispersing to ensure the particle size of the white carbon black after drying, and performing spray drying or flash drying: so that the white carbon black keeps fine spherical particle size and larger specific surface area.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
Example 1
The aluminum fluoride byproduct fluorine-containing silicon slag produced by a company in Hubei is used as a raw material, and the technical indexes are as follows:
SiO2: 60.3% (dry basis); NSA: 28m2/g。
1, deacidifying, homogenizing and pulping the dispersed material
Deacidifying the fluorine-containing silicon slag material separated by the vacuum belt filter with a centrifuge (or directly feeding the fluorine-containing silicon slag separated by the vacuum belt filter into a homogenizing kettle), and weighing the H-containing silicon slag after deacidification2SiF6Feeding 300Kg of material with the liquid amount of 50% into a 1000L homogenizing stirring tank, adding tap water for pulping, controlling the concentration of the pulp at 30%, controlling the stirring speed at 2000-2300r/min, sampling into a pear-shaped separating funnel for observation after 300min to form stable suspension, and measuring the pH value of the suspension to be 2 by using a precision test paper. The slurry is sent into a plate-and-frame filter press and a centrifuge for combined dehydration, and then is put into a homogenizing kettle, tap water is added into the homogenizing kettle to enable the slurry to be a stable suspension liquid with the concentration of about 30 percent, and the slurry is pulped for 80 min. And then is ready for use.
2, ultrasonic fine washing
And (2) feeding the material obtained in the step (1) into an ultrasonic washing device, adding tap water to prepare 10% slurry concentration, washing at the temperature of 45 ℃, controlling the ultrasonic frequency of 60KHz, performing ultrasonic treatment for 100min, then dehydrating, washing for 3 times repeatedly in the way, and then washing for 3 times by using pure water for later use.
3, pulping and spray drying
And (3) adding pure water into the material obtained in the step (2) by using a homogenizing kettle, stirring into 20% of stable suspension slurry according to the stirring speed in the step (1), and then sending into a spray dryer for drying, wherein the dried material is high-quality white carbon black. Through detection: SiO 22: 92.6% (dry basis); NSA: 201g/m2Total iron content: 0.0051% and oil absorption number (DBP) of 3.3cm3/g。
Example 2
The aluminum fluoride byproduct fluorine-containing silicon slag produced by a company in Hubei is used as a raw material, and the technical indexes are as follows:
SiO2: 55.8% (dry basis); NSA: 30m2/g。
1, deacidifying, homogenizing, pulping and dispersing
300Kg of fluorine-containing silicon slag material (containing H) separated by the vacuum belt filter is weighed2SiF6Liquid amount is 60%) is added with tap water in a homogenizing kettle for pulping, the concentration of the pulp is controlled at 25%, the stirring speed is controlled at 2500-2800r/min, the time is 240min, a sample is taken to a pear-shaped separating funnel for observation, a stable suspension is formed, and the pH value is measured to be 2 by a precision test paper. Then dewatering, putting the dewatered material into a homogenizing kettle, adding tap water to make the slurry concentration be 20%, starting a beater to beat for 60min, and sampling and observing to form stable suspension. Then dehydrating for later use.
2, ultrasonic fine washing
And (2) feeding the material obtained in the step (1) into an ultrasonic washing device, adding tap water to prepare 20% slurry concentration, controlling the ultrasonic frequency to be 80KHz at 55 ℃, carrying out ultrasonic treatment for 80min, then dehydrating, washing for 3 times repeatedly in the way, then washing for 3 times by using pure water, and dehydrating for later use.
3, homogenizing, pulping and spray drying
Adding pure water into the material obtained in the step 2 by using a homogenizing kettle, and stirring the mixture to 15 percent according to the stirring speed in the step 1Forming stable suspension liquid by slurry, and then sending the suspension liquid into a spray dryer for drying, wherein the dried material is high-quality white carbon black. Through detection: SiO 22: 95.6% (dry basis); NSA: 229g/m2Total iron content: 0.0031% and an oil absorption number (DBP) of 3.6cm3/g。
Example 3
The aluminum fluoride byproduct fluorine-containing silicon slag produced by a company in Hubei is used as a raw material, and the technical indexes are as follows:
SiO2: 40.8% (dry basis); NSA: 21m2/g
1, centrifugal deacidification, homogeneous beating and dispersion
Weighing 300Kg of fluorine-containing silicon slag (containing H) after centrifugal deacidification of silicon slag material2SiF6The liquid amount is 53 percent), the mixture is put into a homogenizing kettle, tap water is added for pulping, the concentration of the pulp is controlled to be 10 percent, the stirring speed is controlled to be 3000-3200r/min, the time is 180min, then the mixture is sampled into a pear-shaped separating funnel for observation, stable suspension is formed, and the pH value is measured to be 2 by using precision test paper. Then dewatering, putting the dewatered material into a homogenizing kettle, adding tap water to make the slurry concentration be 30%, starting a beater, beating at the same rotating speed for 45min, and then keeping for later use.
2, ultrasonic treatment
And (3) feeding the material obtained in the step (2) into an ultrasonic washing device, controlling the ultrasonic frequency to be 100KHz at the temperature of 65 ℃, carrying out ultrasonic treatment for 60 minutes, dehydrating, repeatedly carrying out ultrasonic washing for 3 times in the way, then carrying out ultrasonic washing for 3 times by using pure water, and dehydrating for later use.
3, homogenizing, pulping and spray drying
And (3) adding pure water into the material obtained in the step (2) in a homogenizing kettle, beating the material into 10% slurry suspension, carrying out ultrasonic treatment for 30min, and then sending the slurry suspension into a spray dryer for drying, wherein the dried material is high-quality white carbon black. Through detection: SiO 22: 96.1% (dry basis); NSA: 226g/m2(ii) a Total iron content: 0.0040%; oil absorption number (DBP) of 3.4cm3/g。
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (7)
1. A method for directly preparing high-purity white carbon black by using fluorine-containing silicon slag is characterized by comprising the following steps:
(1) firstly, carrying out homogenizing pulping and dispersing on fluorine-containing silicon slag to ensure that aluminum hydroxide powder wrapped in solid white carbon black particles is dispersed to react with fluosilicic acid adsorbed by the solid white carbon black to generate an aluminum fluoride solution dissolved in water and a solid silicon dioxide material;
(2) removing acid liquor containing aluminum fluoride, and carrying out at least one time of homogenizing pulping, dispersing and ultrasonic fine washing on the obtained solid silicon dioxide material until washing water is neutral;
(3) and dehydrating and drying the neutral silicon dioxide material to obtain the high-quality white carbon black.
2. The method according to claim 1, wherein the deacidification treatment in the step (2) is carried out by adopting a plate-and-frame filter press and a centrifuge.
3. The method according to claim 1, wherein the pulping process is performed using a homogenizing kettle.
4. The method according to claim 1, characterized in that tap water or pure water is adopted for beating, the concentration of the slurry is controlled to be 10-30%, and the beating time is 3-5 h.
5. The method according to claim 1, wherein in the ultrasonic fine washing process, tap water or pure water is adopted to prepare the materials into slurry with the concentration of 10% -30%, the temperature is 45-65 ℃, and the ultrasonic treatment time is 60-100 min.
6. The method of claim 1, wherein the neutral silica material of step (3) is subjected to homogenization beating after dehydration and before drying.
7. The method of claim 1, wherein the dehydrated silica material is spray or flash dried.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111762790A (en) * | 2020-07-07 | 2020-10-13 | 锦洋高新材料股份有限公司 | Novel method for modifying white carbon black |
| CN113371720A (en) * | 2021-07-16 | 2021-09-10 | 昆明理工大学 | Method for preparing white carbon black by adding sulfuric acid into fluorine-containing silicon slag through dry impurity removal |
| CN113461021A (en) * | 2021-07-16 | 2021-10-01 | 昆明理工大学 | Method for extracting white carbon black from fluorine-containing silicon slag through sulfur-adding wet purification |
| CN113620304A (en) * | 2021-09-09 | 2021-11-09 | 无锡恒诚硅业有限公司 | Preparation method of hydrophobic white carbon black |
| CN114477197A (en) * | 2022-03-11 | 2022-05-13 | 瓮福（集团）有限责任公司 | Method for preparing white carbon black by microwave plasma torch |
| CN115784239A (en) * | 2022-06-24 | 2023-03-14 | 科顺防水科技股份有限公司 | Preparation method of white carbon black |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111762790A (en) * | 2020-07-07 | 2020-10-13 | 锦洋高新材料股份有限公司 | Novel method for modifying white carbon black |
| CN113371720A (en) * | 2021-07-16 | 2021-09-10 | 昆明理工大学 | Method for preparing white carbon black by adding sulfuric acid into fluorine-containing silicon slag through dry impurity removal |
| CN113461021A (en) * | 2021-07-16 | 2021-10-01 | 昆明理工大学 | Method for extracting white carbon black from fluorine-containing silicon slag through sulfur-adding wet purification |
| CN113620304A (en) * | 2021-09-09 | 2021-11-09 | 无锡恒诚硅业有限公司 | Preparation method of hydrophobic white carbon black |
| CN113620304B (en) * | 2021-09-09 | 2024-02-23 | 无锡恒诚硅业有限公司 | Preparation method of hydrophobic white carbon black |
| CN114477197A (en) * | 2022-03-11 | 2022-05-13 | 瓮福（集团）有限责任公司 | Method for preparing white carbon black by microwave plasma torch |
| CN115784239A (en) * | 2022-06-24 | 2023-03-14 | 科顺防水科技股份有限公司 | Preparation method of white carbon black |
| CN115784239B (en) * | 2022-06-24 | 2024-03-19 | 科顺防水科技股份有限公司 | Preparation method of white carbon black |
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