CN114539811A - High-covering-performance easily-dispersible silica fume and preparation method thereof - Google Patents

High-covering-performance easily-dispersible silica fume and preparation method thereof Download PDF

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CN114539811A
CN114539811A CN202210192873.1A CN202210192873A CN114539811A CN 114539811 A CN114539811 A CN 114539811A CN 202210192873 A CN202210192873 A CN 202210192873A CN 114539811 A CN114539811 A CN 114539811A
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coating
silica fume
silicon powder
aluminum
slurry
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田林
林琳
杨振
杨妮
庄晓东
李小英
彭学斌
闫森
刁微之
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Kunming Metallurgical Research Institute
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Abstract

The invention discloses high-covering easy-dispersing silica fume and a preparation method thereof. The high-covering easy-dispersing silica fume is characterized in that the covering power of the high-covering easy-dispersing silica fume is more than 60%, and the high-covering easy-dispersing silica fume is prepared by taking silica fume particles as raw materials through the steps of pretreatment, zirconium coating, aluminum coating and post-treatment. The preparation method comprises the steps of pretreatment, zirconium coating, aluminum coating and post-treatment. The high-covering easy-dispersing silica fume is suitable for the fields of common coating, rubber, plastics, paper making and the like, the covering rate of titanium dioxide is more than 60%, the silica fume has certain dispersibility, and the modified silica fume completely or partially replaces the fields of common coating, rubber, plastics, paper making and the like according to the requirements of the application fields.

Description

High-covering-performance easily-dispersible silica fume and preparation method thereof
Technical Field
The invention belongs to the technical field of metallurgy, and particularly relates to high-covering easy-to-disperse silica fume and a preparation method thereof.
Background
The micro silicon powder is a large amount of SiO with strong volatility produced in an 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 low covering power and poor dispersibility can occur when the silica fume produced by industry 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.
Titanium dioxide is an important inorganic chemical pigment, and the main component is titanium dioxide. The titanium dioxide powder has important application in the industries of paint, printing ink, paper making, plastic rubber, chemical fiber, ceramic and the like, but the titanium dioxide powder is expensive, and is often only partially added when being used as the paint, so that the quality of some high-end products is influenced. If the surface of the micro silicon powder can be modified and then completely or partially used for replacing titanium dioxide, the product cost can be greatly reduced, and the current situation of solid waste of the micro silicon powder can be changed.
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-covering coated modified micro silicon powder, which can effectively improve the high covering performance of the micro silicon powder under the resin system in the fields of coating, plastics, rubber and the like.
The first purpose of the invention is to provide the micro silicon powder with high covering power and easy dispersion; the second purpose is to provide the preparation method of the high-covering easy-to-disperse silica fume.
The first purpose of the invention is realized by that the covering power of the high-covering easy-to-disperse silica fume is more than 60%, and the silica fume is prepared by taking silica fume particles as raw materials and carrying out pretreatment, zirconium coating, aluminum coating and post-treatment steps.
The second object of the present invention is achieved by a method including steps of pretreatment, zirconium coating, 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) 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 zirconium: heating the material b to 60-80 ℃, adding zirconium oxychloride, 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 finishing coating the zirconium film;
C. coating with aluminum: adding an aluminum-containing compound and an acid or an alkali into the slurry c 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 d after the aluminum film coating is finished
D. And (3) post-treatment:
1) carrying out filter pressing and washing on the material d to remove soluble salts to obtain a filter cake e, and drying and crushing the filter cake e to obtain powder f;
2) and (3) carrying out jet milling on the powder f, and simultaneously adding trimethylolpropane to obtain the target product, namely the easily-dispersible silica fume with high coverage.
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. The desalted water is water which is used for removing or reducing strong electrolyte easy to remove to a certain degree, and the residual salt content is 1-5 mg/L.
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 zirconium: and c, heating the slurry in the step b to 60-80 ℃, adding zirconium oxychloride, controlling the adding time to be 10-120 min, continuously stirring for 10-180 min after the adding is finished, adjusting the pH value to 6.5-9.0, curing for 15-60 min, and coating amorphous hydrated zirconium dioxide on the surface of the micro silicon powder particles after the zirconium film is coated.
d. Coating with aluminum: and c, adding an aluminum-containing compound and acid or alkali into the slurry obtained in the step c 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, curing for 15-60 min, and finishing the aluminum film coating. This is a boehmite type hydrated aluminum film coated on the surface of the microsilica particles.
e. 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.
f. 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 several of sodium hexametaphosphate, sodium silicate, carboxylate and isopropanolamine, and the addition amount of the dispersing agent is 1 per mill to 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 concentration of zirconium oxychloride in the step c is 80-140 g/L (ZrO 2)2Calculated by the weight of the micro silicon powder), the adding amount is 0.5-25 percent of the mass of the micro silicon powder (calculated by ZrO)2Meter).
And c, adding zirconium oxychloride and 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.
In the step d, the aluminum-containing compound is aluminum sulfate, sodium metaaluminate and the like, and the concentration of the aluminum-containing compound is 80-280 g/L (by Al)2O3Calculated), the adding amount is 1-15% of the mass of the micro silicon powder (calculated by Al)2O3Meter).
The addition of the aluminum-containing compound and the acid or base in step d is performed in a cocurrent manner (i.e., the aluminum-containing compound is added simultaneously with the acid or base) to keep the pH stable.
And d, adding the aluminum-containing compound and the acid or the alkali into the mixture obtained in the step d, wherein the stirring speed is 250-400 r/min, and the adding time is 10-120 min.
And e, the pressure filtration equipment in the step e is a membrane filter press, a rotary drum filter and the like, and the solid content of a filter cake is more than or equal to 65 percent.
And e, drying equipment in the step e 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 f is superheated steam, compressed air, compressed nitrogen and the like.
And f, adding Trimethylolpropane (TMP) in the step f 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 value of the slurry is mainly adjusted by acid or alkali, and the pH value of the slurry comprises concentrated sulfuric acid (the concentration mass fraction is 98%), hydrochloric acid (the mass fraction is 36.5%), sodium hydroxide (the mass fraction is 50% and 20%) 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 an active hydrous zirconium dioxide film. Pseudo-boehmite type hydrated alumina films and organic films. The active hydrated zirconium dioxide film obviously improves the covering performance of the micro silicon powder. The boehmite type hydrated alumina film and the organic film improve the dispersion performance of the micro silicon powder in the resin.
(2) According to different application fields, the price of the titanium dioxide is 2-4 ten thousand yuan/ton. The particle size morphology of the micro silicon powder is similar to that of titanium dioxide, the chemical property is stable, but the cost of the micro silicon powder is low, and is only 200-300 yuan/ton. The cost of the micro silicon powder subjected to surface modification by the process after industrialization is 2000-3000 yuan/ton, and the cost of subsequent products can be greatly reduced after titanium dioxide is replaced.
(3) The covering power of the modified silica fume with high covering power and high dispersibility prepared by the invention can reach 94.34%, and the modified silica fume has certain dispersibility. The titanium dioxide powder and the filler have the covering rate of over 90 percent and certain dispersibility, and the modified silica fume can completely or partially replace the pigment and filler fields such as titanium white, resin, pigment and filler (kaolin, talcum powder and calcium powder), film-forming agent and additive according to the requirements of the application fields.
(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 high-covering easy-to-disperse silica fume of the present invention;
FIG. 2 is a TEM (Transmission Electron microscope) atlas diagram of the high-covering easy-to-disperse silica fume prepared in example 2 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-covering easy-dispersing silica fume is prepared by taking silica fume particles as raw materials through the steps of pretreatment, zirconium coating, aluminum coating and post-treatment, wherein the covering power of the high-covering easy-dispersing silica fume is more than 60%.
The preparation method of the high-covering easy-to-disperse silica fume comprises the steps of pretreatment, zirconium coating, 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) 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 zirconium: heating the material b to 60-80 ℃, adding zirconium oxychloride, 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 finishing coating the zirconium film;
C. coating with aluminum: adding an aluminum-containing compound and an acid or an alkali into the slurry c 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 d after the aluminum film coating is finished
D. And (3) post-treatment:
1) carrying out filter pressing and washing on the material d to remove soluble salts to obtain a filter cake e, and drying and crushing the filter cake e to obtain powder f;
2) and (3) carrying out jet milling on the powder f, and simultaneously adding trimethylolpropane to obtain the target easily-dispersed silica fume with high coverage.
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 concentration of the zirconyl chloride in the step B is 80-140 g/L, and the adding amount of the zirconyl chloride is 0.5-25% of the mass of the raw material micro silicon powder particles.
The aluminum-containing compound in the step C 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 1-15% 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)2O5Measured), dispersing for 5min by using an ultrasonic instrument, controlling the power at 400W, placing the mixture in a single-layer glass reaction kettle, heating and stirring the mixture to 70 ℃, slowly adding zirconyl chloride for 30min, adding 100g/L zirconyl chloride solution, wherein the total amount of the zirconyl chloride is ZrO2Calculated as 3.0 percent of the micro silicon powder, sodium hydroxide is slowly added for 30min to adjust the pH value to 7.0, and the mixture is aged for 30min after the addition. Adjusting pH to 7.0 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 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, and adding TMP in the crushing process, wherein the addition amount of TMP is microsilica5 per mill, and crushing to obtain the finished product.
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 ℃. Slowly adding zirconyl chloride for 30min, adding 100g/L zirconyl chloride solution, the total amount of zirconyl chloride is ZrO2Calculated as 10.0 percent of the micro silicon powder, sodium hydroxide is slowly added for 30min to adjust the pH value to 7.5, and the mixture is aged for 30min after the addition. 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, 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 3
Preparing 1L of 350g/L micro silicon powder slurry, and adding 1 ‰ (sodium hexametaphosphate) as P2O5Calculating), dispersing for 10min by using an ultrasonic instrument, controlling the power at 700W, placing in a single-layer glass reaction kettle, heating and stirring to 70 ℃, slowly adding zirconyl chloride for 30min, adding 100g/L zirconyl chloride solution, wherein the total amount of zirconyl chloride is ZrO2Calculated as 15.0 percent of the micro silicon powder, sodium hydroxide is slowly added for 30min to adjust the pH value to 8.0, and the mixture is aged for 30min after the addition. Adjusting pH to 8.0 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 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 using an ultrasonic instrument, controlling the power at 700W, placing in a single-layer glass reaction kettle, heating and stirring to 70 ℃, slowly adding zirconyl chloride for 30min, adding 100g/L zirconyl chloride solution, wherein the total amount of zirconyl chloride is ZrO2Calculated as 20.0 percent of the micro silicon powder, sodium hydroxide is slowly added for 30min to adjust the pH value to 8.5, and the mixture is aged for 30min after the addition. Adjusting pH to 8.5 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 crushing, adding TMP in the crushing process, wherein the addition amount of the TMP is 3 per mill of the micro silicon powder, and obtaining the finished product after crushing.
The finished products of examples 1-4 and the uncoated samples were formulated as hiding power test slurries. The same paint is adopted to prepare a sample into a paint paste according to a certain formula and method, a wet film preparation device is used for preparing a coating film with the same thickness on a covering power test paper, the coating film is naturally dried, a spectrophotometer is adopted to measure samples on a black substrate and a white substrate, and PCQC color quality control system software is used for directly representing the covering power of the sample. The specific test method is as follows:
(1) preparing a lacquer slurry: weighing 100g of glass grinding micro-beads in a glass bottle, weighing 50g of acrylic acid (or alkyd) varnish, placing the acrylic acid (or alkyd) varnish into the bottle, adding 12g of sample, placing the glass bottle filled with the materials into a vibration blending machine, and carrying out vibration grinding for 90 min.
(2) Preparing a coating: and brushing the zirconium white powder paint slurry on the covering power test paper by using a 100-micron wet film preparation device by using an automatic film coater to form a coating film, and airing the coating film at room temperature.
(3) And (3) measuring the covering power: and (3) measuring the white substrate and the black substrate after coating by adopting a CM-2600d spectrophotometer, and directly representing the covering power of the sample by PCQC color quality control system software.
The samples were tested for hiding power according to the dispersion method described above, with higher values for hiding power. The test results are shown in table 1.
TABLE 1
Figure DEST_PATH_IMAGE001

Claims (10)

1. The high-covering easy-dispersing silica fume is characterized in that the covering power of the high-covering easy-dispersing silica fume is more than 60%, and the high-covering easy-dispersing silica fume is prepared by taking silica fume particles as raw materials through the steps of pretreatment, zirconium coating, aluminum coating and post-treatment.
2. The method for preparing the high-covering easy-dispersing micro silicon powder as claimed in claim 1, which comprises the steps of pretreatment, zirconium coating, 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 stirring uniformly to obtain slurry a;
2) 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 zirconium: heating the material b to 60-80 ℃, adding zirconium oxychloride, 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 finishing coating the zirconium film;
C. coating with aluminum: adding an aluminum-containing compound and an acid or an alkali into the slurry c 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 d after the aluminum film coating is finished
D. And (3) post-treatment:
1) carrying out filter pressing and washing on the material d to remove soluble salts to obtain a filter cake e, and drying and crushing the filter cake e to obtain powder f;
2) and (3) carrying out jet milling on the powder f, and simultaneously adding trimethylolpropane to obtain the target easily-dispersed silica fume with high coverage.
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 concentration of zirconyl chloride in step B is 80-140 g/L, and the addition amount is 0.5-25% of the mass of the raw material microsilica particles.
8. The method according to claim 2, wherein the aluminum-containing compound in step C 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 1-15% 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.
CN202210192873.1A 2022-03-01 2022-03-01 High-covering-performance easily-dispersible silica fume and preparation method thereof Pending CN114539811A (en)

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