CN114539810A - High-dispersion modified silica fume and preparation method thereof - Google Patents
High-dispersion modified silica fume and preparation method thereof Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention discloses high-dispersion modified silica fume and a preparation method thereof. The high-dispersion modified silica fume has the dispersibility of below 35 microns and is prepared by taking silica fume particles as raw materials through the steps of pretreatment, aluminum coating and post-treatment. The preparation method comprises the steps of pretreatment, aluminum coating and post-treatment. The dispersibility of the high-dispersion modified silica fume prepared by the invention is below 35 microns. The modified silica fume has dispersing performance below 35 micron and may be used to replace kaolin, talcum powder, barium sulfate, mica powder, wollastonite, attapulgite, light calcium carbonate, heavy calcium carbonate, etc. in common paint, rubber, plastic, etc.
Description
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to high-dispersion modified silica fume and a preparation method thereof.
Background
The silicon micropowder is SiO with strong volatility produced in ore-smelting electric furnace when ferroalloy is used for smelting ferrosilicon and industrial silicon (metallic silicon)2And Si gas, the gas is quickly oxidized, condensed and precipitated with air after being emptied, and the industrial dust is collected by a dust collector. The industrial dust mainly contains SiO2Carrying with K2O、Na2O、Ca、F2O3、Al2O3And the like. The silica fume can be widely applied to the fields of concrete, metallurgical pelletizing auxiliary agents, refractory materials, cement materials and the like at present, but the added value of the applied product is not high, and the silica fume basically belongs to the forced consumption of solid wastes. A large amount of micro silicon powder is generated when industrial silicon and ferrosilicon are produced in some places in Yunnan, 2 ten thousand tons of micro silicon powder are generated in an accumulated way every year, and the micro silicon powder is nearly waste because the price of the micro silicon powder is low, the geographical position of a plant is remote, and the micro silicon powder does not have a market, so that the occupied land and the environment are polluted.
The particle size of the silica fume is usually between 0.2 and 5 mu m, and the silica fume is suitable for the fields of pigments and fillers such as coating, plastics, papermaking, rubber and the like, but the problem of poor dispersibility can occur when the industrially produced silica fume is directly used for the fields of coating, plastics, papermaking, rubber and the like. Therefore, the research on the high-value utilization of the modified micro silicon powder is of great significance.
Disclosure of Invention
Aiming at the defects of the existing micro silicon powder processing technology and production technology, the invention provides a preparation method of coated micro silicon powder, in particular to a preparation method of high-dispersion coated modified micro silicon powder, which can effectively improve the dispersion performance of the micro silicon powder in resin systems in the fields of coating, plastics, rubber and the like.
The first purpose of the invention is to provide a high-dispersion modified silica fume; the second purpose is to provide the preparation method of the high-dispersion modified silica fume.
The first purpose of the invention is realized by that the high-dispersion modified silica fume with the dispersibility below 35 microns is prepared by taking silica fume particles as raw materials through the steps of pretreatment, aluminum coating and post-treatment.
The second object of the present invention is achieved by a method including steps of pretreatment, aluminum coating, and post-treatment, including:
A. pretreatment:
1) preparing micro silicon powder slurry: adding the raw material micro silicon powder particles into desalted water to prepare slurry, adjusting the pH value of the slurry to 6.5-9, adding a dispersing agent, and uniformly stirring to obtain slurry a;
2) ultrasonic dispersion: placing the slurry a in an ultrasonic instrument to completely disperse the aggregate of the micro silicon powder particles to present the primary particle state to obtain a material b;
B. coating with aluminum: adding an aluminum-containing compound and acid or alkali into the slurry b at the same time, keeping the pH value stable at 6.5-9 within 10-120 min, continuously stirring for 10-180 min after the addition is finished, adjusting the pH value to 6.5-9.0, and curing for 15-60 min to obtain a material c after aluminum film coating;
D. and (3) post-treatment:
1) carrying out filter pressing and washing on the material c to remove soluble salts to obtain a filter cake d, and drying and crushing the filter cake d to obtain powder e;
2) and (3) carrying out jet milling on the powder e, and simultaneously adding trimethylolpropane to obtain the target high-dispersion modified silica fume.
The specific operation method comprises the following steps:
a. preparing micro silicon powder slurry: adding the micro silicon powder particles into desalted water to prepare slurry, adjusting the pH value of the slurry to 6.5-9, and adding a dispersing agent.
b. Ultrasonic dispersion: and (b) putting the slurry obtained in the step (a) into an ultrasonic instrument, and controlling ultrasonic power and ultrasonic time to completely disperse the aggregate of the micro silicon powder particles to present the primary particle state.
c. Coating with aluminum: adding an aluminum-containing compound and acid or alkali into the slurry b at the same time, keeping the pH value stable at 6.5-9 within 10-120 min, continuously stirring for 10-180 min after the addition is finished, adjusting the pH value to 6.5-9.0, and curing for 15-60 min to complete aluminum film coating to obtain a material c;
d. filter pressing, washing and drying: and d, performing filter pressing and washing on the slurry obtained in the step d, removing soluble salts in the slurry to enable the resistivity of the filter cake to be larger than or equal to 80 omega-m, drying the filter cake at 85-350 ℃, and crushing the filter cake into powder.
e. Organic coating and crushing: and e, carrying out steam flow crushing on the micro silicon powder obtained in the step e, and simultaneously adding Trimethylolpropane (TMP) to obtain a final product.
The concentration of the micro silicon powder base material slurry in the step a is 250 g/L-500 g/L.
The dispersing agent in the step a is one or a combination of more of sodium hexametaphosphate, sodium silicate, carboxylate and isopropanolamine, and the addition amount of the dispersing agent is 1-9 per mill of the content of the micro silicon powder.
And c, controlling the power of the ultrasonic instrument in the step b to be 300-1000W, and controlling the ultrasonic time to be 2-20 min.
And c, controlling the particle size distribution D (50) of the micro silicon powder particles subjected to ultrasonic dispersion in the step b to be 0.30-0.60 mu m.
The aluminum-containing compound in the step c is aluminum sulfate, sodium metaaluminate or the like, and the concentration of the aluminum-containing compound is 80g/L to 280g/L (by Al)2O3Calculated by Al), the adding amount is 0.5-5 percent of the mass of the micro silicon powder (calculated by Al)2O3Meter).
Containing aluminium compounds and acids or bases in step c aboveThe addition is carried out in cocurrent flow (i.e. the aluminium-containing compound is mixed with an acid or a base) Simultaneously add)And the pH value is kept stable.
And c, adding the aluminum-containing compound and the acid or the alkali into the mixture in the step c, wherein the stirring speed is 250-400 r/min, and the adding time is 10-120 min.
The pressure filtration equipment in the step d is a diaphragm filter press, a rotary drum filter and the like, and the solid content of the filter cake is more than or equal to 65 percent.
And d, drying equipment in the step d is a box type drying box and a flash evaporation dryer, and the water content after drying is less than or equal to 0.2%.
The carrier pulverized by steam flow in the step e is superheated steam, compressed air, compressed nitrogen and the like.
And e, adding Trimethylolpropane (TMP) in the step e in an amount of 1-20 per mill of the mass of the micro silicon powder in an inlet or outlet of a steam flow pulverizer.
The pH of the slurry is mainly adjusted by acid-base compounds, including concentrated sulfuric acid (with the concentration of 98 mass percent), hydrochloric acid (with the mass percent of 36.5 percent), sodium hydroxide (with the mass percent of 50 percent and 20 percent) and the like.
The invention has the beneficial effects that:
(1) the surface of the micro silicon powder prepared by the invention is coated with a pseudo-boehmite type hydrated alumina film and an organic film. The boehmite type hydrated alumina film and the organic film improve the dispersion performance of the micro silicon powder in the resin.
(2) The dispersibility of the high-dispersion modified silica fume prepared by the invention is below 35 microns. The modified silica fume has dispersing performance below 40 micron and may be used to replace kaolin, talcum powder, calcium powder and other stuffing in common paint, rubber, plastic, paper and other fields.
(3) The market price of the fillers in the current market, such as kaolin, talcum powder and calcium carbonate, is about 2000 yuan/ton, the industrialization cost of the modified silica fume by the process is 500 yuan/ton and 800 yuan/ton, and the cost of subsequent products can be greatly reduced by using the modified silica fume as the fillers.
(4) The process flow is simple, and industrialization is easy to realize.
Drawings
FIG. 1 is a schematic process flow diagram of a preparation method of highly dispersed modified silica fume of the present invention;
FIG. 2 is a schematic TEM (Transmission Electron microscope) spectrum of the highly dispersed modified silica fume prepared in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples and the accompanying drawings, but the present invention is not limited thereto in any way, and any modifications or alterations based on the teaching of the present invention are within the scope of the present invention.
The high-dispersion modified silica fume has the dispersibility of below 35 microns and is prepared by taking silica fume particles as raw materials through the steps of pretreatment, aluminum coating and post-treatment.
The preparation method of the high-dispersion modified silica fume comprises the steps of pretreatment, aluminum coating and post-treatment, and comprises the following steps:
A. pretreatment:
1) preparing micro silicon powder slurry: adding the raw material micro silicon powder particles into desalted water to prepare slurry, adjusting the pH value of the slurry to 6.5-9, adding a dispersing agent, and uniformly stirring to obtain slurry a;
2) ultrasonic dispersion: placing the slurry a in an ultrasonic instrument to completely disperse the aggregate of the micro silicon powder particles to present the primary particle state to obtain a material b;
B. coating with aluminum: adding an aluminum-containing compound into the material b, adjusting the pH value to 6.5-9.0, controlling the pH value to be stable at 6.5-9.0 within 10-120 min, continuously stirring for 10-180 min, adjusting the pH value to 6.5-9.0, and curing for 15-60 min to obtain a material c after aluminum film coating;
D. and (3) post-treatment:
1) carrying out filter pressing and washing on the material c to remove soluble salts to obtain a filter cake d, and drying and crushing the filter cake d to obtain powder e;
2) and (3) carrying out jet milling on the powder e, and simultaneously adding trimethylolpropane to obtain the target high-dispersion modified silica fume.
The desalted water in the step A1) is water with strong electrolyte easy to remove removed or reduced to a certain degree, and the residual salt content is 1-5 mg/L.
The dispersing agent in the step A1) is one or more of sodium hexametaphosphate, sodium silicate, carboxylate and isopropanolamine, and the adding amount of the dispersing agent is 1-9 per mill of the mass of the raw material micro silicon powder particles.
The concentration of the slurry a in the step 1) is 250-500 g/L.
The power of the ultrasonic instrument in the step A2) is 300-1000W, and the ultrasonic time is 2-20 min.
The particle size distribution of the material b in the step A is 0.30-0.60 mu m.
In step B saidThe aluminum-containing compound is aluminum sulfate or sodium metaaluminate, and the concentration of the aluminum-containing compound is Al2O3The amount of the added silica micro powder is 80-280 g/L, and the added amount is 0.5-5% of the mass of the raw material silica micro powder particles.
And D) the carrier for airflow pulverization in the step 2) is superheated steam, compressed air or compressed nitrogen.
D, adding the trimethylolpropane into the micro silicon powder particles in the step 2) in an amount which is 1-20 per mill of the mass of the micro silicon powder particles, wherein the adding mode is an inlet or an outlet of a jet mill.
The invention is further illustrated by the following specific examples:
example 1
Preparing 1L of 350g/L micro silicon powder slurry, and adding 1 per mill of sodium hexametaphosphate (P)2O5Dispersing for 5min by an ultrasonic instrument, controlling the power at 400W, placing in a single-layer glass reaction kettle, heating and stirring to 70 ℃, adjusting the pH value to 7.0 by using sulfuric acid, always keeping the pH value within the range of plus or minus 0.5 fluctuation during the process of adding sodium metaaluminate, adding a sodium metaaluminate solution with the concentration of 150g/L, wherein the total amount of the sodium metaaluminate is Al2O3Calculated as 3.0 percent of the micro silicon powder, namely 70mL, the flow rate is 4.67mL/min, and the mixture is aged for 30min after the addition is finished. Adjusting pH to 6.8 with sulfuric acid, and aging for 30 min. Then filter pressing and washing, drying at 105 ℃, then adopting airflow for crushing, adding TMP in the crushing process, wherein the addition of the TMP is 5 per mill of the micro silicon powder, and obtaining the finished product after crushing.
Example 2
Preparing 1L of 350g/L micro silicon powder slurry, and adding 1 per mill of sodium hexametaphosphate (P)2O5Calculating), dispersing for 8min by an ultrasonic instrument, controlling the power at 600W, placing in a single-layer glass reaction kettle, heating and stirring to 70 ℃. Adjusting pH to 7.5 with sulfuric acid, and adding 150g/L sodium metaaluminate solution with total amount of aluminum metaaluminate (Al) within + -0.5 of pH fluctuation during sodium metaaluminate addition2O3Calculated as 2.5 percent of the micro silicon powder, namely 58.3mL, the flow rate is 3.89mL/min, and the mixture is aged for 15min after the addition. Adjusting pH to 7.0 with sulfuric acid, and aging for 15 min. Then filter pressing and washing, drying at 105 ℃, then adopting airflow for crushing, and adding in the crushing processAdding TMP, wherein the addition amount of the TMP is 5 per mill of the micro silicon powder, and crushing to obtain the finished product.
Example 3
Preparing 1L of 350g/L micro silicon powder slurry, and adding 1 per mill of sodium hexametaphosphate (P)2O5Calculating), dispersing for 10min by an ultrasonic instrument, controlling the power at 700W, placing in a single-layer glass reaction kettle, heating and stirring to 70 ℃, adjusting the pH value to 8.0 by using sulfuric acid, always keeping the pH value within the range of plus or minus 0.5 fluctuation during the process of adding sodium metaaluminate, adding 150g/L sodium metaaluminate solution, wherein the total amount of the metaaluminate is Al2O3Calculated as 3.0 percent of the micro silicon powder, namely 70mL, the flow rate is 4.67mL/min, and the mixture is aged for 15min after the addition is finished. Adjusting pH to 7.0 with sulfuric acid, and aging for 15 min. Then filter pressing and washing, drying at 105 ℃, then adopting airflow for crushing, adding TMP in the crushing process, wherein the addition of the TMP is 5 per mill of the micro silicon powder, and obtaining the finished product after crushing.
Example 4
Preparing 1L of 350g/L micro silicon powder slurry, and adding 1 per mill of sodium hexametaphosphate (P)2O5Calculating), dispersing for 15min by an ultrasonic instrument, controlling the power at 700W, placing in a single-layer glass reaction kettle, heating and stirring to 70 ℃, adjusting the pH value to 8.5 by using sulfuric acid, always keeping the pH value within the range of plus or minus 0.5 fluctuation during the process of adding sodium metaaluminate, adding 150g/L sodium metaaluminate solution, wherein the total amount of the metaaluminate is Al2O3Calculated as 2.5 percent of the micro silicon powder, namely 58.3mL, the flow rate is 3.89mL/min, and the mixture is aged for 15min after the addition. Adjusting pH to 7.0 with sulfuric acid, and aging for 15 min. Then filter pressing and washing, drying at 105 ℃, then adopting airflow for crushing, adding TMP in the crushing process, wherein the addition of the TMP is 3 per mill of the micro silicon powder, and obtaining the finished product after crushing.
The finished products and the uncoated samples in the examples 1-4 are prepared into dispersion detection slurry, 3.0000g of the sample is weighed and placed in the middle of a lower glass plate of a flat grinding instrument, and 2.8000g of standard slurry is respectively extracted by two syringes. Firstly adding 2.8000g of standard slurry, uniformly mixing the standard slurry by using a knife, completely smearing the knife on an upper glass plate, applying a force of 1KN, grinding twice, each time rotating for 25 times, collecting the slurry in the middle of the glass plate by using the knife once for grinding, adding 2.8000g of standard slurry after grinding, uniformly mixing the standard slurry and the slurry by using the knife, and collecting the slurry in the glossy paper for later use. A sufficient amount of sample is dropped into the deep end of the groove of the blade gauge and the sample is allowed to overflow slightly (several drops of sample are dropped, so that the groove is filled slightly more than necessary). Note that the sample is representative, and not so much that the sample entrains air bubbles, which appear on the gauge as particles, can affect the observation of fineness. The scraper is held between a thumb and a forefinger of two hands, the edge of the scraper is lifted to the deepest end of the groove of the fineness gauge and is in contact with the surface of the fineness gauge, the scraper is perpendicular to the surface of the fineness gauge, the scraper is enabled to scrape from the deep part to the shallow part of the groove at a uniform speed within 1-2 seconds, enough pressure is applied to the scraper so that the groove is filled with a sample, and redundant slurry is scraped.
The gauge was observed from the side within 3 seconds after scraping, in a manner such that the line of sight was at an angle of 20-30 ° to the plane of the groove, while observing under light that readily viewed the condition of the sample in the groove. Attention should be paid to observation immediately after scraping, and the result accuracy is affected by the phenomenon of thickening due to overlong time. The sample was observed at the point where dense particles first appeared, and the position where more than 5 particles appeared in a band having a width of 3 mm across the groove was determined as a dispersion fineness value reading point.
The samples were tested for dispersibility according to the dispersion method described above, with larger values giving poorer dispersibility. The test results are shown in table 1.
TABLE 1
Claims (10)
1. The high-dispersion modified silica fume is characterized in that the high-dispersion modified silica fume has the dispersibility of below 35 microns and is prepared by taking silica fume particles as raw materials through the steps of pretreatment, aluminum coating and post-treatment.
2. The method for preparing the highly dispersed modified silica fume as claimed in claim 1, which comprises the steps of pretreatment, aluminum coating and post-treatment, and comprises the following steps:
A. pretreatment:
1) preparing micro silicon powder slurry: adding the raw material micro silicon powder particles into desalted water to prepare slurry, adjusting the pH value of the slurry to 6.5-9, adding a dispersing agent, and uniformly stirring to obtain slurry a;
2) ultrasonic dispersion: placing the slurry a in an ultrasonic instrument to completely disperse the aggregate of the micro silicon powder particles to present the primary particle state to obtain a material b;
B. coating with aluminum: adding an aluminum-containing compound and acid or alkali into the slurry b at the same time, keeping the pH value stable at 6.5-9 within 10-120 min, continuously stirring for 10-180 min after the addition is finished, adjusting the pH value to 6.5-9.0, and curing for 15-60 min to complete aluminum film coating to obtain a material c;
D. and (3) post-treatment:
1) carrying out filter pressing and washing on the material c to remove soluble salts to obtain a filter cake d, and drying and crushing the filter cake d to obtain powder e;
2) and (3) carrying out jet milling on the powder e, and simultaneously adding trimethylolpropane to obtain the target high-dispersion modified silica fume.
3. The method according to claim 2, wherein the desalted water in step a 1) is water from which strong electrolyte that is easily removed is removed or reduced to a certain extent, and the remaining salt content is 1 to 5 mg/L.
4. The preparation method according to claim 2, wherein the dispersant in the step A) is one or more of sodium hexametaphosphate, sodium silicate, carboxylate and isopropanolamine, and the addition amount is 1-9 per mill of the mass of the raw material micro silicon powder particles.
5. The preparation method according to claim 2, wherein the concentration of the slurry a in the step A1) is 250-500 g/L.
6. The preparation method according to claim 2, wherein the power of the ultrasonic instrument in the step A2) is 300-1000W, and the ultrasonic time is 2-20 min.
7. The preparation method according to claim 2, wherein the particle size distribution of the material b in the step A is 0.30-0.60 μm.
8. The process according to claim 2, wherein the aluminum-containing compound in step B is aluminum sulfate or sodium metaaluminate, and the concentration of the aluminum-containing compound is Al2O3The amount of the added silica micro powder is 80-280 g/L, and the added amount is 0.5-5% of the mass of the raw material silica micro powder particles.
9. The method according to claim 2, wherein the carrier for jet milling in step D2) is superheated steam, compressed air or compressed nitrogen.
10. The preparation method according to claim 2, wherein the trimethylolpropane in the step D2) is added in an amount of 1-20 per mill of the mass of the raw material micro silicon powder particles, and the adding mode is an inlet or an outlet of a jet mill.
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