CN109942002B - Depolymerization method of silicon dioxide microspheres in by-product silica fume for producing zirconium oxide - Google Patents
Depolymerization method of silicon dioxide microspheres in by-product silica fume for producing zirconium oxide Download PDFInfo
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Abstract
A method for depolymerizing silicon dioxide microspheres in by-product silica fume generated in zirconia production is characterized in that ZrO is produced by an electric melting method2SiO in by-product silica fume2The property and agglomeration characteristic of the microspheres provide a method for producing ZrO by an electric melting method2SiO in by-product silica fume2The invention relates to a method for depolymerizing microspherical particles, which mainly comprises the following steps: preparing a silica fume powder-water suspension, and performing alkali dissolution treatment, washing silica fume-alkali dissolution products, grinding and dispersing agents by using a silica fume-alkali dissolution product grinder medium, and filtering and drying the silica fume-grinding products on the silica fume powder-water suspension; the method solves the problem of producing ZrO by an electric melting method2SiO in by-product silica fume2The microspheres are seriously agglomerated and are difficult to realize stable dispersion, thereby improving the production of ZrO by an electric melting method2The service performance and the utilization value of the by-product silica fume are used for generating SiO2And the controlled agglomeration is realized in the particle process.
Description
The technical field is as follows:
the method relates to the technical field of depolymerization of silica microspheres in silica fume which is a byproduct in zirconia production, in particular to a treatment method for depolymerization of silica microspheres in silica fume which is a byproduct in zirconia production.
Background art:
the silica fume involved in the method is a byproduct in the industrial production of zirconium oxide by an electric smelting method. The structural formula of the zirconium oxide is ZrO2It has high melting point, strong chemical stability, acid resistance, alkali resistance and reducibility, thus becoming one of the important basic raw materials for the development of modern high-tech industry. ZrO can be produced by adopting two methods of chemical synthesis and electric melting2In which the electric melting method produces ZrO2The process of (1) is as follows: is composed of zirconium silicate (ZrSiO)4The zircon is taken as a raw material, carbon is taken as a reducing agent, a proper amount of catalyst or stabilizer is added, and ZrSiO is finally subjected to the high-temperature action of an electric arc furnace4Decomposition into ZrO2And silicon dioxide. The chemical formula of the silicon dioxide is SiO2Due to SiO formed2Reduction by carbon to SiO, i.e. the escape of SiO gas, and thus ZrO can be separated therefrom2And (5) producing the product. SiO gas is oxidized into amorphous SiO when meeting cold air in the process of exhausting from a flue2And becomes silica fume as a by-product. Due to oxidation of SiO to SiO2For the rapid condensation process, Si and O atoms are not in time to form an ordered arrangement, so that SiO is formed2Cannot be crystalline but can only be amorphous, and form spherical particles with the size of micron order. Due to high temperature, SiO2The microspheres have stronger bonding effect, so an agglomerated form is formed. In addition, the silica fume also contains a small amount of ZrO2And (4) components.
Silica fume is generally used as solid waste for piling treatment in the past, occupies land and causes resource waste. In recent years, SiO based on silica fume has2High purity, strong activity of volcanic ash on particle surface and good fluidity, and the volcanic ash can be partially applied as an admixture or additive of cement, concrete and refractory material products, but has limited functional effectThe added value of the product is lower. In addition, the silica fume has high whiteness, and SiO in the silica fume2The microspheres have high hardness, strong surface activity, uniform size and good fluidity, and the characteristics make the processing of the silica fume into the excellent functional filler possible. However, SiO in silica fume2The microspheres have the problem of serious interparticle agglomeration, and the prior art conditions are difficult to realize effective depolymerization and dispersion. Therefore, in practical applications, SiO is generally used2The microsphere aggregate is directly applied as an additive raw material. The agglomeration phenomenon of the silica microspheres restricts the effective exertion of the volcanic ash activity of the silica microspheres and simultaneously becomes an obstacle for preparing the functional filler, so that the problems of uneven dispersion in a matrix, reduced use performance and the like in the application process are caused. Thus, the technical means is adopted to lead SiO in the silica fume2The microsphere aggregate is effectively depolymerized, secondary aggregation is prevented, and the method plays an important role in improving the reaction activity and the utilization efficiency of the microsphere aggregate and expanding the field of high value-added products.
The agglomeration between solid particles can be classified into soft agglomeration and hard agglomeration according to a formation mechanism, wherein the soft agglomeration refers to the agglomeration formed by weak bonding action of micro-nano particles, such as van der waals force and electrostatic force, and the agglomeration is easy to break up. While hard agglomeration mainly refers to aggregation with strong bonding action formed by the formation of hydrogen bonds, crystal bridges, chemical bonds and surface atom diffusion between particles. In an electric melting process ZrO2SiO in the produced by-product silica fume2The micro-spheroids have both hard and soft agglomeration, i.e. are first formed by SiO2The unit particles are aggregated by hard agglomeration to form secondary particles having a strong interparticle binding force, and then re-aggregated by soft agglomeration of the secondary particles with each other. Therefore, SiO in the silica fume2The deagglomeration of microsphere agglomerates must be carried out to address these characteristics.
Since hard agglomeration between solid particles occurs mainly during the preparation of the particles, preventing the particles from forming agglomerates in the preparation process is a major measure to eliminate the problem of hard agglomeration. Such as in the preparation of titanium dioxide (TiO)2) In the process of nano-particle, ethanol-containing mixed solvent is used, surfactant is added or the product is stored inHard agglomeration can be prevented by controlling the agglomeration of particles in solvents and the like, which are inefficient, have limited controllability, and do not control agglomeration of particles as a by-product.
Technical scheme
The method aims at solving the problem of producing ZrO by an electric melting method2SiO in by-product silica fume2The agglomeration of the microspheres is serious, and the stable dispersion is difficult to realize.
For improving the production of ZrO by electrofusion2The service performance and the utilization value of the by-product silica fume are solved, and the problem that the by-product silica fume is difficult to generate SiO2The problems of agglomeration and the like are controlled in the particle process, and the invention produces ZrO by an electric melting method2SiO in by-product silica fume2The property and agglomeration characteristic of the microspheres provide a method for producing ZrO by an electric melting method2SiO in by-product silica fume2The invention relates to a method for depolymerizing microspherical particles, which mainly comprises the following steps: preparing a silica fume powder-water suspension, and performing alkali dissolution treatment on the silica fume powder-water suspension, washing the silica fume-alkali dissolution product, grinding the silica fume-alkali dissolution product by using a grinder medium and dispersing a dispersing agent, and filtering and drying the silica fume-ground product.
Realizing the production of ZrO by an industrial electric melting method2SiO in by-product silica fume2The specific method and the steps for depolymerizing the microspheres are as follows:
preparation of silica fume powder-water suspension: the silica fume powder and water are weighed according to the weight percentage of 20-50 percent of silica fume powder and 50-80 percent of water, mixed and put into a stirrer to be stirred at high speed for 30-40min to prepare the silica fume powder-water suspension.
(II) alkali dissolution treatment of silica fume powder-water suspension: selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches the range of 11-13, and continuously stirring for 20-30 min to obtain the silica fume-alkali solution product suspension.
(III) washing the silica fume-alkali soluble product with water: and (3) filtering the silica fume-alkali soluble product suspension prepared in the step (II) in a three-leg centrifuge or a plate-and-frame filter press to obtain a filter cake, then adding water into the filter cake in a high-speed stirrer, stirring for 20-30 min, and filtering the suspension, wherein the water washing is regarded as 1 time. The stirring and water washing steps were repeated 3 times.
(IV) grinding the silica fume-alkali soluble product by using a grinder medium and dispersing a dispersing agent: selecting sodium silicate as a dispersing agent, adding 50-80% of water and 0.5% of sodium silicate solution into the filter cake washed for 3 times according to the step (three), stirring for 15-20 min to obtain a suspension, placing the suspension into a vertical stirring mill or a horizontal sand mill, adding mullite balls accounting for 2-3 times of the weight of the silica fume and having the diameter of 1-3mm, and stirring and grinding for 30-45 min;
(V) silica fume-ground product filtration drying: filtering the ground silica fume-water suspension obtained in the step (IV) to obtain a filter cake, and drying the filter cake in an oven, or directly drying the silica fume-water suspension by using a flash evaporation dryer to obtain ZrO produced by an electric melting method2SiO in by-product silica fume2The microspheres depolymerize and disperse the product.
Preferably, the step (a) is the preparation of the silica fume powder-water suspension: weighing the silica fume and water according to the weight percentage of 35 percent of silica fume powder and 65 percent of water, mixing and placing in a stirrer to stir at high speed for 35min to prepare the silica fume powder-water suspension.
Preferably, the alkali-soluble treatment of the silica fume powder-water suspension of the step (II): and (2) selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches 12.5, and continuously stirring for 20min to obtain the silica fume-alkali solution product suspension.
Preferably, the silica fume-alkali solution product obtained in the step (three) is washed by water: placing the silica fume-alkali solution product suspension prepared in the step (II) into a plate-and-frame filter press for filtering to obtain a filter cake, then placing the filter cake into a high-speed stirrer, adding water for stirring for 20min, and then filtering the suspension by using the plate-and-frame filter press, wherein the water washing is regarded as 1 time; the stirring and water washing steps were repeated 3 times.
Preferably, the silica fume-alkali dissolution product mill media milling and dispersant dispersion of step (iv): selecting sodium silicate as a dispersing agent, adding 59.8 percent of water and 0.2 percent of sodium silicate solution into the filter cake obtained by washing for 3 times according to the step (three), stirring for 20min to obtain a silica fume-water suspension, placing the suspension into a vertical stirring mill, and adding a mixture of silica fume: 2: 3mm of mullite balls with the ratio of 2:3:5, and stirring and grinding for 40 min.
Further, the step (I) of preparing the silica fume powder-water suspension comprises the following steps: the silica fume powder-water suspension is prepared by weighing silica fume and water according to the weight percentage of 25 percent of silica fume powder and 75 percent of water, mixing and placing in a stirrer to stir at high speed for 40 min.
Further, the alkali dissolution treatment of the silica fume powder-water suspension in the step (II): and (2) selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches 11.5, and continuously stirring for 25min to obtain the silica fume-alkali solution product suspension.
Further, the silica fume-alkali solution product obtained in the step (III) is washed by water: putting the silica fume-alkali solution suspension prepared in the step (II) into a three-foot centrifuge for filtering to obtain a filter cake, then putting the filter cake into a high-speed stirrer, adding water for stirring for 25min, and then filtering the suspension by using the three-foot centrifuge, wherein the suspension is treated as water washing for 1 time; the above stirring and water washing steps were repeated 3 times.
Further, the silica fume-alkali solution product grinder medium grinding and dispersant dispersing of the step (IV): adding 64.825% of water and sodium silicate solution accounting for 0.175% of the weight of the silica fume into the filter cake washed for 3 times according to the step (three), stirring for 20min to obtain silica fume-water suspension, placing the suspension into a vertical stirring mill, and adding the mixture accounting for 2.5 times of the weight of the silica fume in the suspension, wherein the diameter of the mixture is 1: 2: 3mm of mullite beads with the ratio of 2:3:5, and stirring and grinding for 35 min.
The innovativeness and the principle of the invention are described as follows: (1) the alkali solution treatment process of the silica fume aqueous suspension comprises the following steps: production of ZrO by electrofusion2Among the by-product silica fume, SiO alone2The microspheres are generally strongly bonded by dehydroxylation to form Si-O-Si bonds and thus aggregated into secondary particles of hard agglomerated nature. Feeding the aqueous silica fume suspensionThe alkali dissolution treatment can break or weaken Si-O-Si bonds through reaction with-OH, thereby eliminating or reducing the acting force between primary particles and creating conditions for depolymerization. The specific reaction is as follows: Si-O-Si + OH- → Si-OH + Si-O-; (2) and (3) grinding the aqueous silica fume suspension medium after alkali dissolution: in SiO2On the basis that the bonding force among the microsphere particles is weakened, the impact, the shearing and the stripping of the grinding medium are used for overcoming the defects of SiO2The bonding force among the microspheres realizes SiO in the silica fume2And (4) depolymerizing the microspheres. (3) Function of the dispersant: in the aqueous silica fume-suspension, alkali dissolving, medium grinding to make SiO2On the premise of realizing depolymerization of the microspheres, sodium silicate serving as a dispersant is added to prevent depolymerized SiO2The microsphere particles are agglomerated again.
Detailed Description
The method for depolymerizing the silica microspheres in the byproduct silica fume generated in the production of zirconia is realized, and the specific implementation mode is as follows:
example 1:
the depolymerization treatment object is the industrial electric melting method for producing ZrO2By-product silica fume, chemical composition SiO thereof2An amorphous phase. The silica fume is white powder and consists of micron-sized spherical particles with the primary particle size of 0.5-3 mu m and the particle size D of the thick end9018.551 μm, median diameter D502.582 μm.
Production of ZrO by electric melting method2SiO in by-product silica fume2The microsphere depolymerization process comprises the following steps:
preparation of silica fume powder-water suspension: weighing the silica fume and water according to the weight percentage of 35 percent of silica fume powder and 65 percent of water, mixing and placing in a stirrer to stir at high speed for 35min to prepare the silica fume powder-water suspension.
(II) alkali dissolution treatment of silica fume powder-water suspension: and (2) selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches 12.5, and continuously stirring for 20min to obtain the silica fume-alkali solution product suspension.
(III) washing the silica fume-alkali soluble product with water: and (3) filtering the silica fume-alkali solution product suspension prepared in the step (II) in a plate-and-frame filter press to obtain a filter cake, then placing the filter cake in a high-speed stirrer, adding water, stirring for 20min, and filtering the suspension in the plate-and-frame filter press, wherein the washing is regarded as 1 time. The stirring and water washing steps were repeated 3 times.
(IV) grinding the silica fume-alkali soluble product by using a grinder medium and dispersing a dispersing agent: selecting sodium silicate as a dispersing agent, adding 59.8 percent of water and 0.2 percent of sodium silicate solution into the filter cake obtained by washing for 3 times according to the step (three), stirring for 20min to obtain a silica fume-water suspension, placing the suspension into a vertical stirring mill, and adding a mixture of silica fume: 2: 3mm of mullite balls with the ratio of 2:3:5, and stirring and grinding for 40 min;
(V) silica fume-ground product filtration drying: filtering the ground silica fume-water suspension obtained in the step (IV), drying a filter cake by using an oven to obtain ZrO produced by the electric melting method2SiO in by-product silica fume2The microspheres depolymerize and disperse the product.
Example 2:
the depolymerization treatment object is the industrial electric melting method for producing ZrO2By-product silica fume, chemical composition SiO thereof2An amorphous phase. The silica fume is white powder and consists of micron-sized spherical particles with the primary particle size of 0.5-3 mu m and the particle size D of the thick end9018.551 μm, median diameter D502.582 μm.
Production of ZrO by electric melting method2SiO in by-product silica fume2The microsphere depolymerization process comprises the following steps:
preparation of silica fume powder-water suspension: the silica fume powder-water suspension is prepared by weighing silica fume and water according to the weight percentage of 25 percent of silica fume powder and 75 percent of water, mixing and placing in a stirrer to stir at high speed for 40 min.
(II) alkali dissolution treatment of silica fume powder-water suspension: and (2) selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches 11.5, and continuously stirring for 25min to obtain the silica fume-alkali solution product suspension.
(III) washing the silica fume-alkali soluble product with water: and (3) filtering the silica fume-alkali solution product suspension prepared in the step (II) in a three-foot centrifuge to obtain a filter cake, then placing the filter cake in a high-speed stirrer, adding water, stirring for 25min, and filtering the suspension by the three-foot centrifuge, wherein the suspension is washed by water for 1 time. The above stirring and water washing steps were repeated 3 times.
(IV) grinding the silica fume-alkali soluble product by using a grinder medium and dispersing a dispersing agent: adding 64.825% of water and sodium silicate solution accounting for 0.175% of the weight of the silica fume into the filter cake washed for 3 times according to the step (three), stirring for 20min to obtain silica fume-water suspension, placing the suspension into a vertical stirring mill, and adding the mixture accounting for 2.5 times of the weight of the silica fume in the suspension, wherein the diameter of the mixture is 1: 2: 3mm of mullite balls with the ratio of 2:3:5, and stirring and grinding for 35 min;
(V) silica fume-ground product filtration drying: directly drying the ground silica fume-water suspension obtained in the step (IV) by using a flash evaporation dryer to obtain ZrO produced by an electric melting method2SiO in by-product silica fume2The microspheres depolymerize and disperse the product.
Production of ZrO by electrofusion methods prepared in examples 1 and 2, respectively2SiO in by-product silica fume2The main particle size indices of the microsphere deagglomeration and dispersion products are given in Table 1, and the coarse end particle size (D) of the silica fume after deagglomeration and dispersion90) Is close to SiO2The grain diameter of the microsphere primary particles is 0.5-3 mu m.
Table particle size distribution of silica fume once deagglomerated and dispersed
The foregoing description is of the best mode contemplated for carrying out the inventive concepts and principles of operation. The above embodiments should not be construed as limiting the inventive concept and the working principle, and other embodiments and implementations and combinations of embodiments and implementations according to the inventive concept belong to the scope of protection of the present invention.
Claims (9)
1. A method for depolymerizing silicon dioxide in silica fume as a byproduct of zirconia production, comprising the steps of:
preparation of silica fume powder-water suspension: weighing 20-50 wt% of silica fume powder and 50-80 wt% of water, mixing, stirring at high speed for 30-40min in a stirrer to obtain silica fume powder-water suspension;
(II) alkali dissolution treatment of silica fume powder-water suspension: selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches the range of 11-13, and continuously stirring for 20-30 min to obtain a silica fume-alkali solution suspension;
(III) washing the silica fume-alkali soluble product with water: placing the silica fume-alkali soluble product suspension prepared in the step (II) into a three-leg centrifuge or a plate-and-frame filter press for filtering to obtain a filter cake, then placing the filter cake into a high-speed stirrer, adding water, stirring for 20-30 min, filtering the suspension, regarding as washing for 1 time, and repeating the stirring and washing steps for 3 times;
(IV) grinding the silica fume-alkali soluble product by using a grinder medium and dispersing a dispersing agent: selecting sodium silicate as a dispersing agent, adding 50-80% of water and 0.5% of sodium silicate solution into the filter cake washed for 3 times according to the step (three), stirring for 15-20 min to obtain a suspension, placing the suspension into a vertical stirring mill or a horizontal sand mill, adding mullite balls accounting for 2-3 times of the weight of the silica fume and having the diameter of 1-3mm, and stirring and grinding for 30-45 min;
(V) silica fume-ground product filtration drying: filtering the ground silica fume-water suspension obtained in the step (IV) to obtain a filter cake, and drying the filter cake in an oven, or directly drying the silica fume-water suspension by using a flash evaporation dryer to obtain ZrO produced by an electric melting method2SiO in by-product silica fume2The microspheres depolymerize and disperse the product.
2. The method of claim 1, wherein: the preparation of the silica fume powder-water suspension in the step (I): weighing the silica fume and water according to the weight percentage of 35 percent of silica fume powder and 65 percent of water, mixing and placing in a stirrer to stir at high speed for 35min to prepare the silica fume powder-water suspension.
3. The method of claim 1, wherein: the second step is alkali dissolution treatment of the silica fume powder-water suspension: and (2) selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches 12.5, and continuously stirring for 20min to obtain the silica fume-alkali solution product suspension.
4. The method of claim 1, wherein: and (3) washing the silica fume-alkali solution product: placing the silica fume-alkali solution product suspension prepared in the step (II) into a plate-and-frame filter press for filtering to obtain a filter cake, then placing the filter cake into a high-speed stirrer, adding water for stirring for 20min, and then filtering the suspension by using the plate-and-frame filter press, wherein the water washing is regarded as 1 time; the stirring and water washing steps were repeated 3 times.
5. The method of claim 1, wherein: the silica fume-alkali dissolution product grinder medium grinding and dispersant dispersing in the step (IV): selecting sodium silicate as a dispersing agent, adding 59.8 percent of water and 0.2 percent of sodium silicate solution into the filter cake obtained by washing for 3 times according to the step (three), stirring for 20min to obtain a silica fume-water suspension, placing the suspension into a vertical stirring mill, adding mullite balls accounting for 3 times of the weight of silica fume, wherein the ratio of the mullite balls with the diameter of 1mm, 2mm and 3mm is 2:3:5, and stirring and grinding for 40 min.
6. The method of claim 1, wherein: the preparation of the silica fume powder-water suspension in the step (I): the silica fume powder-water suspension is prepared by weighing silica fume and water according to the weight percentage of 25 percent and 75 percent of water, mixing and placing in a stirrer to stir at high speed for 40 min.
7. The method of claim 1, wherein: the second step is alkali dissolution treatment of the silica fume powder-water suspension: and (2) selecting sodium hydroxide as an alkali treatment agent, slowly adding a sodium hydroxide solution with the concentration of 20% into the silica fume powder-water suspension prepared in the step (1), stirring, measuring the pH value of the solution, stopping adding the sodium hydroxide solution when the pH value of the suspension reaches 11.5, and continuously stirring for 25min to obtain the silica fume-alkali solution product suspension.
8. The method of claim 1, wherein: and (3) washing the silica fume-alkali solution product: putting the silica fume-alkali solution suspension prepared in the step (II) into a three-foot centrifuge for filtering to obtain a filter cake, then putting the filter cake into a high-speed stirrer, adding water for stirring for 25min, and then filtering the suspension by using the three-foot centrifuge, wherein the suspension is treated as water washing for 1 time; the above stirring and water washing steps were repeated 3 times.
9. The method of claim 1, wherein: the silica fume-alkali dissolution product grinder medium grinding and dispersant dispersing in the step (IV): adding 64.825% of water and a sodium silicate solution accounting for 0.175% of the weight of the silica fume into the filter cake washed for 3 times according to the step (three), stirring for 20min to obtain a silica fume-water suspension, placing the suspension into a vertical stirring mill, adding mullite balls accounting for 2.5 times of the weight of the silica fume, wherein the ratio of the mullite balls with the diameter of 1mm, 2mm and 3mm is 2:3:5, and stirring and grinding for 35 min.
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