CN116022798A - Preparation method for preparing high-dispersity white carbon black by taking fluosilicic acid as raw material - Google Patents
Preparation method for preparing high-dispersity white carbon black by taking fluosilicic acid as raw material Download PDFInfo
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Abstract
The invention belongs to the technical field of powder material preparation, and particularly relates to a preparation method for preparing high-dispersity white carbon black by taking fluosilicic acid as a raw material. The preparation method for preparing the high-dispersity white carbon black by taking fluosilicic acid as a raw material comprises the following steps: and adding a pore-enlarging agent in the reaction process of the fluosilicic acid solution and the ammonia water solution, and after the reaction is finished, carrying out solid-liquid separation and drying to obtain the high-dispersity white carbon black product. The white carbon black prepared by the invention has good dispersibility, moderate specific surface area, higher pore volume and oil absorption value, can be used in the field of tires, has simple and stable whole process and low cost, has low requirement on equipment, and can be used for mass production.
Description
Technical Field
The invention belongs to the technical field of powder material preparation, and particularly relates to a preparation method for preparing high-dispersity white carbon black by taking fluosilicic acid as a raw material.
Background
White carbon black is also called hydrated silicon dioxide, and has a molecular formula of SiO 2 ·nH 2 O can be divided into precipitation white carbon black and gas phase white carbon black according to different preparation processes. The white carbon black has the advantages of good chemical stability, good electrical insulation, high dispersibility, high specific surface area and the like, can be applied to more than ten fields of plastics, rubber, papermaking, paint, dye, printing ink and the like, and particularly has high dispersibility requirement on the white carbon black in the field of rubber tires. The white carbon black prepared by the gas phase method process has remarkable technical advantages due to the advantages of small crystal grains (less than or equal to 20 nm), less agglomeration and the like. However, the process takes silicon tetrachloride, oxygen and hydrogen as raw materials, and prepares white carbon black (SiCl) by reaction at high temperature 4 +2H 2 +O 2 →SiO 2 +4HCl), the preparation process has the problems of high energy consumption, high cost, poor production safety and the like, and limits the large-scale application of the white carbon black in the field of tires. Due to precipitation (H) 2 SiF 6 +6NH 4 OH＝6NH 4 F+SiO 2 ·nH 2 O, n=4) has the advantage of lower cost, so the synthesis of the high-dispersion white carbon black is a focus of attention at home and abroad by taking a precipitation method as a basic process and improving and optimizing the technology.
As a byproduct of phosphate ores with larger domestic storage capacity, the high-value utilization of low-grade fluosilicic acid resources is concerned by technical workers at home and abroad. At present, fluosilicic acid is used as a raw material, and products such as basic fluochemical raw materials hydrofluoric acid, silicon tetrafluoride, fluoride salt cryolite for aluminum, aluminum fluoride and the like can be developed and are successfully applied to production practice. The technology for preparing industrial raw material hydrogen fluoride from fluosilicic acid can be further divided into three types according to raw materials: fluosilicic acid (or sodium fluosilicate) -sulfuric acid method, fluosilicic acid-potassium fluoride medium method and silicon tetrafluoride-water vapor gas phase method, wherein white carbon black by-product precipitation method can be prepared in the latter two processes, and patents and documents on white carbon black preparation are reported. Because the white carbon black is produced by precipitation in a liquid phase, the existence of hydroxyl on the surface of the white carbon black can promote the agglomeration of the white carbon black, and the high dispersion performance cannot be obtained and the white carbon black can not be applied to the tire industry; in addition, fluosilicic acid contains fluoride ions with strong electronegativity and oxygen ions in white carbon black, so that the silicon ions and the fluoride ions compete for combination effect, and crystallization and self-dispersibility of the white carbon black are affected. Therefore, developing a high-dispersibility white carbon black product by taking low-grade fluosilicic acid with high fluosilicic acid separation difficulty as a raw material becomes a challenge.
Next, the specific surface area of the white carbon black was measured by a nitrogen adsorption method. The principle is that small molecular nitrogen molecules enter the white carbon black pores, and the specific surface area is obtained by measuring the nitrogen adsorption amount of the white carbon black. Micropores (less than 2 nm) and mesopores (2 nm-50 nm) are key for obtaining the self-height ratio of the white carbon black, macropores (more than 50 nm) are key for realizing uniform dispersion of the white carbon black in rubber, the higher the macropore pore volume is, the faster the permeation rate of rubber molecules is, the better the dispersibility of the white carbon black is, and meanwhile, the obtained oil absorption value is higher (more than 2 cm) 3 /g). The white carbon black synthesis process and the additive are taken as an improvement method, and the key point of synergistically obtaining the white carbon black with proper specific surface area and high dispersion is that the pore structure of the white carbon black is regulated and controlled.
National standard HG/T3061-2009 prescribes that the BET value of the specific table of high-dispersity precipitated hydrated silicon dioxide is more than or equal to 191m 2 The ratio of the total of the components per gram is not less than 300m 2 And/g, the white carbon black is poor in dispersibility in rubber, and local agglomeration is caused. For example, chinese patent No. CN104828832A discloses a method for preparing high-dispersity white carbon black by hydrochloric acid precipitation, and the specific surface area of the white carbon black obtained by the method is 392-426 m 2 Per gram, the pore volume is 1.6-1.7 cm 3 And/g. Although the patent obtains higher specific surface area, the pore volume is smaller (< 2 cm) 3 And/g), the dispersibility in rubber tires is poor, and the usability of white carbon black is affected.
Disclosure of Invention
The invention aims to provide a preparation method for preparing high-dispersibility white carbon black by taking fluosilicic acid as a raw material, so as to solve the problem of poor dispersibility when the white carbon black prepared in the prior art is applied to rubber tires due to mismatch of specific surface area and oil absorption value.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method for preparing high-dispersity white carbon black by taking fluosilicic acid as a raw material comprises the following steps:
and adding a pore-enlarging agent in the reaction process of the fluosilicic acid solution and the ammonia water solution, and after the reaction is finished, carrying out solid-liquid separation and drying to obtain the high-dispersity white carbon black product.
According to the invention, the low-grade fluosilicic acid is used as a silicon source, ammonia water is used as a dissociation agent, the white carbon black is synthesized, compared with the dissociation agents such as aluminum hydroxide, concentrated sulfuric acid and the like, the ammonia water has the most obvious effect of improving the fluosilicic acid separation efficiency, and the pore structure of the white carbon black can be enriched by introducing the pore-expanding agent. The specific surface area of the high-dispersion white carbon black prepared by the invention is 150-300 m 2 Per gram, the oil absorption value is 2.4-3.2 cm 3 And (3) the dispersion is good, and the modified polyurethane can be used in the field of tires. The invention has simple and stable process, lower cost and lower requirement on equipment performance, and can be used for large-scale production.
Preferably, the reaction is to drop fluosilicic acid solution into ammonia water solution, monitor system pH in the reaction process, and add pore expanding agent when the system pH reaches 8-10.
The pH of the initial ammonia water is 12, the pH of the system is reduced by the added fluosilicic acid, when the pH reaches 8-10, partial white carbon black crystal grains are formed, and a pore expanding agent is introduced and fully mixed with the white carbon black crystal grains. The addition time of the pore-expanding agent is mainly that a certain amount of white carbon black powder is in the system, and the interval is 30-40 wt.%. When the pore-expanding agent is added, the fluosilicic acid is stopped from being added, and if the fluosilicic acid solution is continuously added, the fluosilicic acid solution reacts with the pore-expanding agent immediately, so that the pore-expanding effect is affected.
Preferably, the pore-expanding agent is added when the pH of the system reaches 8.5-9.0.
Preferably, the pore-expanding agent is a soluble aluminum salt. The fineness and the proportion of the pore-expanding agent are as follows: 30 to 40wt.% of 0.5 to 10 μm, 30 to 40wt.% of 10 to 44 μm and 30 to 40wt.% of 44 to 100 μm; the pore-expanding agent is added by uniformly mixing and then introducing. The fineness of the pore-expanding agent has larger influence on the using effect of the pore-expanding agent, and the finer the fineness is, the easier the pore-expanding agent is dissolved in the system, and micropores and mesopores are easier to form. The coarser the fineness, the easier the macropores are formed, and the higher the oil absorption value is. Therefore, white carbon black products with different pore structures can be obtained by adjusting the fineness of the pore-expanding agent.
The pore-expanding agent is introduced to enrich the pore structure of the white carbon black, and the pore-expanding principle is different according to the different pore-expanding agents. The reaming mechanism of the soluble aluminum salt is flocculation precipitation crystallization, the process is that aluminum ions dissolved in the system can be combined with OH in ammonia water - The ions combine to form Al (OH) which is easily precipitated 3 The colloid is slowly flocculated and precipitated between pH values of 7-9, newly generated white carbon black particles (less than 20 nm) are enriched on the surface of flocculate to form agglomerates with about 1 mu m, and then precipitation is carried out, and pores among the agglomerates are macropores, which is the reason for improving the oil absorption value of the white carbon black by soluble aluminum salt.
The requirements for the pore-expanding agent are as follows: 1) The pore-expanding agent should have an obvious pore-expanding effect. Generating gas or forming seed crystal or whisker in situ in the system, providing a growth platform for newly generated white carbon black particles in the form of a template agent, and forming agglomerates composed of large and small grains, wherein macropores among the agglomerates are key for obtaining a high oil absorption value; 2) The fineness of the pore-expanding agent is required, and the pore structures formed by the pore-expanding agent are different in size. The specific surface area test of the white carbon black is to use small molecule N 2 Filled into the pore structure of the white carbon black, so that the higher the volumes of micropores (< 2 nm) and mesopores (between 2nm and 50 nm) are, the higher the volume of the white carbon black is, and the higher the volume of the white carbon black is, and the higher the volume of the white carbon black is, the higher the 2 The more molecules, the higher the specific surface area value obtained.
Preferably, the addition amount of the pore-expanding agent is 5-20 wt.% of the mass of the theoretical design white carbon black product.
In order to ensure that the pore-expanding agent is fully mixed with the system after being added, the pore-expanding agent fully plays a role in expanding pores and improves the pore volume of the white carbon black, preferably, the pore-expanding agent is aged after being added, and the aging time is 0.5-3 h.
Preferably, the fluorosilicic acid solution is continuously added dropwise to react to the end point after the ageing. The aging aims to fully dissociate the pore-expanding agent, stay in the partially synthesized white carbon black structure, and then react with the mixture to generate CO 2 The gas and reaming effect is obvious.
In the whole reaction process, the fluosilicic acid solution is added dropwise, and the dropping speed is 1-20 g/min. Further, the dripping is carried out under stirring, and when the fluosilicic acid solution is dripped before the pore-expanding agent is added, the stirring speed is 200-500 r/min, so that the materials are uniformly mixed, and the reaction speed is improved; after ageing, when the fluosilicic acid solution is added dropwise, the stirring speed is 500-800 r/min, so that part of the obtained white carbon black can be fully scattered under the shearing stirring, the primary grain size and pore structure of the white carbon black can be conveniently controlled, and agglomeration is avoided.
In order to improve the dispersion effect of the white carbon black, a dispersing agent is also added into the aqueous ammonia solution of the priming solution, wherein the dispersing agent is a special dispersing agent for the white carbon black, the dispersing agent is any one of polyethylene glycol, polypropylene ammonium salt, polycarboxylic acid ammonium salt or polyethylene, and the adding amount of the dispersing agent is 10-30 wt.% of the mass of the theoretically designed white carbon black product.
Preferably, the concentration of the fluosilicic acid solution is 10-21%, and the concentration of the ammonia water solution is 2-20 mol/L. The theoretical molar ratio of fluosilicic acid to ammonia is 1:6, and ammonia is excessively introduced in consideration of volatilization of ammonia.
Preferably, the reaction comprises, in addition to the reaction under stirring: the reaction is carried out in a microchannel reactor.
Preferably, the reaction temperature is 20 to 60 ℃.
Preferably, the pH of the system is monitored during the reaction, and when the pH of the system is 5-7, the reaction is completed; further, when the pH of the system is 6.0 to 6.5, the reaction is completed.
Detailed Description
The technical scheme of the invention is further described below with reference to specific embodiments.
1. The specific examples of the preparation method of the high-dispersity white carbon black by taking fluosilicic acid as a raw material are as follows:
example 1
The preparation method of the high-dispersity white carbon black by taking fluosilicic acid as the raw material in the embodiment is according to H 2 SiF 6 +6NH 4 OH＝6NH 4 F+SiO 2 ·nH 2 O, n=4 stoichiometric formula, the theoretical design prepares 100g of white carbon black product, the preparation process includes the following steps:
(1) 2mol/L ammonia water (1000 mL, theoretical 1.68mol/L, considering volatilization of ammonia water, so that ammonia water is slightly excessively introduced) is taken as a priming solution in a reaction container, 20g (20 wt.% of the mass of a white carbon black product is theoretically designed) of white carbon black special dispersant polyethylene glycol (molecular weight 950-1500, 1000 in this example and commercially available conventional products) is added, after full mixing, a fluosilicic acid solution with the concentration of 10% is added dropwise to the solution, the dropping speed is 1g/min, stirring and heating are started, the stirring speed is set to 200r/min, and the synthesis temperature is 20 ℃. When the pH in the solution reaches 9.0, stopping adding the fluosilicic acid solution, and introducing a soluble aluminum salt (aluminum sulfate in the embodiment) of a pore-expanding agent, wherein the addition amount of the soluble aluminum salt is 10g (10 wt.% of the mass of the white carbon black product in theoretical design), and the fineness and the proportion of the pore-expanding agent are as follows: 30wt.% 0.5 μm, 40wt.% 44 μm and 30wt.% 60 μm, are introduced after homogeneous mixing; stopping stirring and aging for 1h.
(2) And (3) after ageing, stirring at a high speed of 800r/min, and simultaneously continuously dropwise adding the fluosilicic acid solution to react at 20 ℃ until the end point, wherein the pH value of the end point of the reaction is 6.5.
The amount of fluorosilicic acid solution with the concentration of 10% is 2410g dropwise during the whole reaction. After the reaction is finished, carrying out suction filtration and filter cake washing, and drying for 3 hours at 120 ℃ to obtain 98g of white carbon black product, wherein the specific surface area of the white carbon black product is 195m 2 Per g, oil absorption value 2.7cm 3 And/g, good dispersibility in rubber.
Example 2
The preparation method for preparing the high-dispersibility white carbon black by taking fluosilicic acid as a raw material in the embodiment theoretically designs and prepares 100g of white carbon black product, and the preparation process comprises the following steps:
(1) 20mol/L ammonia water (11.9L) is used as a priming solution in a reaction container, 30g (30 wt.% of the mass of a white carbon black product in theoretical design) of special dispersing agent polycarboxylic acid ammonium salt of white carbon black (commercially available conventional product) is added, after full mixing, a fluosilicic acid solution with the concentration of 21% is dropwise added into the solution, the dropwise adding speed is 10g/min, stirring and heating are simultaneously started, the stirring speed is set to 500r/min, and the synthesis temperature is 50 ℃. When the pH in the solution reaches 8.5, stopping adding the fluosilicic acid solution, and introducing a soluble aluminum salt (aluminum chloride in the embodiment) of a pore-expanding agent, wherein the addition amount of the soluble aluminum salt is 20g (20 wt.% of the mass of the white carbon black product in theoretical design), and the fineness and the proportion of the pore-expanding agent are as follows: 10 μm 40wt.%, 30 μm 30wt.% and 50 μm 30wt.%, are introduced after homogeneous mixing; stopping stirring and aging for 1h.
(2) And (3) after ageing, stirring at a high speed of 500r/min, and simultaneously continuously dropwise adding the fluosilicic acid solution to react at 50 ℃ until the end point, wherein the pH value of the end point of the reaction is 6.3.
The fluorosilicic acid solution with the concentration of 21% is dripped into 1147g during the whole reaction process. After the reaction is finished, carrying out suction filtration and filter cake washing, and drying at 120 ℃ for 3 hours to obtain 104g of white carbon black product, wherein the specific surface area of the white carbon black product is 240m 2 Per g, oil absorption value 3.1cm 3 And/g, good dispersibility in rubber.
Example 3
The preparation method for preparing the high-dispersibility white carbon black by taking fluosilicic acid as a raw material in the embodiment theoretically designs and prepares 100g of white carbon black product, and the preparation process comprises the following steps:
(1) 15mol/L ammonia water (8.92L) is used as a priming solution in a reaction container, 15g (15 wt.% of the mass of a white carbon black product in theoretical design) of special dispersing agent ammonium polyacrylate for white carbon black (commercially available conventional product) is added, after the mixture is fully mixed, a fluosilicic acid solution with the concentration of 17% is dropwise added into the solution, the dropwise adding speed is 5g/min, stirring and heating are simultaneously started, the stirring speed is set to 400r/min, and the synthesis temperature is 60 ℃. When the pH in the solution reaches 8.8, stopping adding the fluosilicic acid solution, and introducing a soluble aluminum salt (aluminum nitrate in the embodiment) of a pore-expanding agent, wherein the addition amount of the soluble aluminum salt is 5g (5 wt.% of the mass of the white carbon black product in theoretical design), and the fineness and the proportion of the pore-expanding agent are as follows: 35wt.% for 5 μm, 35wt.% for 10 μm and 30wt.% for 70 μm, are introduced after homogeneous mixing; stopping stirring and aging for 1h.
(2) And (3) after ageing, stirring at a high speed of 600r/min, and simultaneously continuously dropwise adding the fluosilicic acid solution to react at 60 ℃ until the end point, wherein the pH value of the end point of the reaction is 6.0.
Dripping fluorine silicon with concentration of 17% in the whole reaction processThe amount of acid solution was 1417g. After the reaction is finished, carrying out suction filtration and filter cake washing, and drying for 3 hours at 120 ℃ to obtain 95g of white carbon black product, wherein the specific surface area of the white carbon black product is 220m 2 Per g, oil absorption value 3.0cm 3 And/g, good dispersibility in rubber.
Example 4
The preparation method for preparing the high-dispersibility white carbon black by taking fluosilicic acid as a raw material in the embodiment theoretically designs and prepares 100g of white carbon black product, and the preparation process comprises the following steps:
(1) 15mol/L ammonia water (8.92L) is taken as a priming solution in a reaction container, 15g (15 wt.% of the mass of a theoretical design white carbon black product) of special dispersant ammonium polyacrylate for white carbon black (commercial conventional product) is added, after the mixture is fully mixed, the mixed solution and a fluosilicic acid solution with the concentration of 17% and the mass of 1417g are introduced into a micro-channel reactor, the reaction temperature is 60 ℃, when the pH value in the reaction solution reaches 8.8, a pore-expanding agent soluble aluminum salt (aluminum nitrate in the embodiment) is introduced into the micro-channel reactor, the addition amount of the pore-expanding agent soluble aluminum salt is 5g, the reaction is continued until the end point, and the pH value of the reaction end point is 6.0.
After the reaction is finished, carrying out suction filtration and filter cake washing, and drying at 120 ℃ for 3 hours to obtain 96g of white carbon black product, wherein the specific surface area of the white carbon black product is 211m 2 Per g, oil absorption value 2.9cm 3 And/g, good dispersibility in rubber.
2. Comparative example
Comparative example 1
The preparation method of the comparative example for preparing the high-dispersibility white carbon black by taking fluosilicic acid as a raw material is basically the same as that of the example 2, except that: whether a pore-expanding agent is introduced.
The preparation method for preparing the high-dispersity white carbon black by taking fluosilicic acid as a raw material in the comparative example is designed and prepared in theory to prepare 100g of white carbon black product, and the preparation process comprises the following steps:
20mol/L ammonia water (11.9L) is used as a priming solution in a reaction container, 30g (30 wt.% of the mass of a theoretical design white carbon black product) of special dispersing agent polycarboxylic acid ammonium salt of white carbon black (commercially available conventional product) is added, after full mixing, 21% fluosilicic acid solution is added dropwise into the solution, the dropping speed is 10g/min, stirring and heating are started, the stirring speed is set to 500r/min, the synthesis temperature is 50 ℃ to the end point, and the pH value of the reaction end point is 6.3.
The fluorosilicic acid solution with the concentration of 21% is dripped into 1147g during the whole reaction process. After the reaction is finished, carrying out suction filtration and filter cake washing, and drying at 120 ℃ for 3 hours to obtain 101g of white carbon black product, wherein the specific surface area of the white carbon black product is 165m 2 Per g, oil absorption value 1.8cm 3 And/g, the dispersibility in rubber is poor.
Comparative example 2
The preparation method of the comparative example for preparing the high-dispersibility white carbon black by taking fluosilicic acid as a raw material is basically the same as that of the example 2, except that: and (3) introducing a pore-expanding agent.
The preparation method for preparing the high-dispersity white carbon black by taking fluosilicic acid as a raw material in the comparative example is designed and prepared in theory to prepare 100g of white carbon black product, and the preparation process comprises the following steps:
(1) 20mol/L ammonia water (11.9L) is used as a priming solution in a reaction container, 30g (30 wt.% of the mass of a white carbon black product in theoretical design) of special dispersing agent polycarboxylic acid ammonium salt of white carbon black (commercially available conventional product) is added, after full mixing, a fluosilicic acid solution with the concentration of 21% is dropwise added into the solution, the dropwise adding speed is 10g/min, stirring and heating are simultaneously started, the stirring speed is set to 500r/min, and the synthesis temperature is 50 ℃. When the pH value in the solution reaches 9.5, stopping adding the fluosilicic acid solution, and introducing a pore-expanding agent soluble aluminum salt (aluminum chloride is adopted in the comparative example), wherein the adding amount of the pore-expanding agent soluble aluminum salt is 20g (20 wt.% of the mass of the white carbon black product in theoretical design), and the fineness and the proportion of the pore-expanding agent are as follows: 10 μm 40wt.%, 30 μm 30wt.% and 50 μm 30wt.%, are introduced after homogeneous mixing; stopping stirring and aging for 1h.
(2) And (3) after ageing, stirring at a high speed of 500r/min, and simultaneously continuously dropwise adding the fluosilicic acid solution to react to a terminal, wherein the pH value of the terminal is 6.3.
The fluorosilicic acid solution with the concentration of 21% is dripped into 1147g during the whole reaction process. After the reaction is finished, carrying out suction filtration and filter cake washing, and drying for 3 hours at 120 ℃ to obtain 104g of white carbon black product, wherein the specific surface area of the white carbon black product is 180m 2 Per g, oil absorption value 1.9cm 3 And/g, the dispersibility in rubber is poor.
Claims (10)
1. The preparation method for preparing the high-dispersity white carbon black by taking fluosilicic acid as a raw material is characterized by comprising the following steps of:
and adding a pore-enlarging agent in the reaction process of the fluosilicic acid solution and the ammonia water solution, and after the reaction is finished, carrying out solid-liquid separation and drying to obtain the high-dispersity white carbon black product.
2. The method for preparing high-dispersibility white carbon black by taking fluosilicic acid as a raw material according to claim 1, wherein the reaction is characterized in that fluosilicic acid solution is dropwise added into ammonia water solution, the pH of a system is monitored in the reaction process, and a pore expanding agent is added when the pH of the system reaches 8-10.
3. The method for preparing high-dispersibility white carbon black by using fluosilicic acid as a raw material according to claim 2, wherein a pore-expanding agent is added when the pH of the system reaches 8.5-9.0.
4. The method for preparing high-dispersibility white carbon black by using fluosilicic acid as a raw material according to claim 1, wherein the pore-expanding agent is a soluble aluminum salt.
5. The method for preparing high-dispersibility white carbon black by taking fluosilicic acid as a raw material according to claim 4, wherein the addition amount of the pore-expanding agent is 5-20 wt.% of the mass of the theoretical design white carbon black product.
6. The method for preparing high-dispersibility white carbon black by using fluosilicic acid as a raw material according to claim 2, wherein the pore-expanding agent is added and then aged for 0.5-3 hours.
7. The method for preparing high-dispersibility white carbon black by using fluosilicic acid as a raw material according to claim 6, wherein the reaction of continuously dropwise adding fluosilicic acid solution to the end point after aging.
8. The method for preparing highly dispersible white carbon black by using fluosilicic acid as a raw material according to claim 1, wherein the concentration of the fluosilicic acid solution is 10-21%, and the concentration of the ammonia water solution is 2-20 mol/L.
9. The method for preparing highly dispersible white carbon black by using fluosilicic acid as a raw material according to claim 1, wherein the reaction is performed in a microchannel reactor.
10. The method for preparing highly dispersible white carbon black by using fluosilicic acid as raw material according to claim 1, wherein the system pH is monitored during the reaction, and when the system pH is 5-7, the reaction is completed.
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