CN109336122B - Preparation method of aluminum silicate - Google Patents
Preparation method of aluminum silicate Download PDFInfo
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- CN109336122B CN109336122B CN201811487477.1A CN201811487477A CN109336122B CN 109336122 B CN109336122 B CN 109336122B CN 201811487477 A CN201811487477 A CN 201811487477A CN 109336122 B CN109336122 B CN 109336122B
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- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
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- C01P2004/00—Particle morphology
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Abstract
The invention relates to a preparation method of aluminum silicate, which comprises the following steps: adding soluble silicate into a solution containing a dispersing agent, preferably dropwise, to form a mixed solution; soluble aluminum salt is added, preferably dropwise, to the resulting mixture to react with the soluble silicate to produce aluminum silicate. The preparation method is simple in preparation process, economic and environment-friendly in process, and the prepared aluminum silicate is small in granularity and good in dispersity.
Description
Technical Field
The invention relates to the field of preparation of materials, in particular to a preparation method of aluminum silicate.
Background
Aluminum silicate is a silicate of the formula Al 2 SiO 5 Since their structure is very complex, they are often written not in the form of salts but in the form of the respective oxides of the metals, i.e. Al 2 O 3 ·SiO 2 . The aluminum silicate has a density of 2.8 to 2.9 g/cc, a refractive index of 1.56, and a mohs hardness that varies between 4.5 and 7.5 depending on the type of ore and the water content.
Aluminium silicates have a wide range of industrial applications. For example, aluminum silicates can be used as fillers for glass, ceramics, pigments, and paints; but also an ideal substitute of titanium dioxide and high-quality kaolin in the coating, and the titanium dioxide and the high-quality kaolin are widely used in the aspects of paint, leather, printing and dyeing, printing ink, paper making, plastics, rubber and the like when being matched with the pigment; the aluminum silicate can also be used for manufacturing high-temperature-resistant fireproof sound-insulation and heat-insulation cotton, plates, pipes, seam felts, fireproof heat-insulation cloth, high-temperature-resistant paper, fireproof heat-insulation ropes, belts, fireproof heat-insulation needled blankets (with throwing and blowing), inorganic fireproof decorative plates, inorganic fireproof rolling curtains and the like; aluminum silicate is also used as a filler for adhesives and sealants, which can improve hardness, whiteness, abrasion resistance, weatherability, and storage stability.
The existing aluminum silicate preparation methods are mostly through a wire throwing method or a blowing method, and the aluminum silicate prepared by the methods is fibrous, so that the prepared aluminum silicate has the defects of uneven length, poor dispersibility and the like.
Disclosure of Invention
In view of the problems of the prior art, it is an object of the present invention to provide a method for producing an aluminum silicate, in which a soluble silicate is added to a solution containing a dispersant, preferably, dropwise, to form a mixed solution, and a soluble aluminum salt is added to the mixed solution, preferably, dropwise, so that the aluminum silicate produced does not contain a fibrous structure, has good dispersibility, and has a small particle size.
The invention provides a preparation method of aluminum silicate, which comprises the following steps:
adding soluble silicate or a part of the soluble silicate to a solution containing a dispersing agent, preferably dropwise, to form a mixed solution;
soluble aluminum salt or the remaining portion of the soluble aluminum salt and the soluble silicate is added, preferably dropwise, to the resulting mixture, thereby reacting the soluble aluminum salt with the soluble silicate to produce aluminum silicate.
The inventor of the application finds that the soluble silicate is added into the solution containing the dispersant preferably and dropwise added, on one hand, the dispersibility of the soluble silicate in the solvent can be improved, so that when the soluble aluminum salt is dropwise added, the soluble silicate can be fully contacted with the soluble aluminum salt, and then fully reacted under the condition of high dispersion, and finally, the prepared aluminum silicate does not contain a fibrous structure, and has better dispersibility and smaller granularity; on the other hand, because the solution contains enough soluble silicate, the soluble aluminum salt can react with the soluble silicate immediately, and the flocculation reaction is avoided.
According to the present invention, in practical operation, in order to reduce the reaction time and improve the reaction efficiency, it is preferable to add a part of the soluble silicate to a solution containing a dispersant, preferably dropwise, to form a mixed solution; the remaining portion of the soluble silicate is then added, preferably dropwise, to the resulting mixture along with a soluble aluminum salt, to react with the soluble silicate to form aluminum silicate.
According to the invention, soluble aluminium salts are added, preferably dropwise, to the obtained mixture, so that they react with the soluble silicate to form a suspension containing aluminium silicate. Then washing the prepared suspension by using deionized water or absolute methanol or absolute ethanol, and drying the washed suspension for 12-16 h at the temperature of 60-110 ℃ to prepare the solid aluminum silicate.
According to the invention, preferably with stirring, soluble silicate is added, preferably dropwise, to the dispersant-containing solution and/or soluble aluminium salt is added, preferably dropwise, to the resulting mixture; more preferably, the stirring operation is performed by a high speed stirring paddle, most preferably, the rotation speed of the high speed stirring paddle is 900-1100rpm; more preferably, the dropwise addition is carried out by a peristaltic pump, and most preferably, the liquid outlet speed of the peristaltic pump is 0.5-3g/min.
According to the present invention, the solution containing the soluble silicate and the solution containing the soluble aluminum salt may be dropped at the same rate or at different rates, preferably at different rates.
According to the present invention, it is preferable to continue stirring for 5 to 20 hours after adding soluble aluminum salt, preferably dropwise, to the obtained mixed solution to make the reaction more sufficient.
In some preferred embodiments of the present invention, the dispersant is selected from at least one of sodium polyacrylate, ammonium polyacrylate, and sodium hexametaphosphate; preferably, the dispersant is sodium polyacrylate.
According to the present invention, the above-mentioned specific dispersant, particularly sodium polyacrylate, has good water solubility and high polarity, and can form soluble chain anions by binding with soluble aluminum salt, and thus is adsorbed on the surface of aluminum silicate solid particles, increasing the charge on the surface of the aggregated solid particles, increasing the repulsion between particles forming steric hindrance, and improving the dispersibility of sodium polyacrylate.
In some preferred embodiments of the present invention, the soluble silicate is selected from at least one of potassium silicate, sodium silicate and ammonium silicate; preferably, the soluble silicate is sodium silicate.
According to the present invention, the potassium silicate, the sodium silicate and the ammonium silicate may be in any conventional form, and for example, the sodium silicate may be anhydrous sodium silicate, sodium silicate pentahydrate, sodium silicate nonahydrate or water glass.
In some preferred embodiments of the present invention, the soluble aluminum salt is selected from at least one of aluminum chloride, aluminum sulfate, aluminum nitrate, and aluminum sulfide; preferably, the soluble aluminium salt is aluminium sulphate.
According to the present invention, aluminum chloride, aluminum sulfate, aluminum nitrate and aluminum sulfide may be used in any conventional form, and for example, anhydrous aluminum sulfate or aluminum sulfate octadecahydrate may be used as aluminum sulfate.
In some preferred embodiments of the present invention, the mass ratio of the soluble silicate to the dispersant is (2-10): 1, preferably (3-8): 1; and/or the mass ratio of the soluble silicate to the soluble aluminium salt is (1-3): 1, preferably (1.8-2.3): 1.
According to the present invention, when the mass ratio of the soluble silicate to the dispersant and/or the mass ratio of the soluble silicate to the soluble aluminum salt is within the above-specified range, it is advantageous to obtain aluminum silicate having a good dispersibility and a small particle size.
In some preferred embodiments of the present invention, the concentration of the dispersant in the dispersant-containing solution is 5% to 30%, preferably 10% to 15%.
According to the invention, in the solution of the dispersant, the solvent is an alcohol organic solvent or water, preferably water; wherein the alcohol organic solution is selected from C 1 -C 5 At least one of the alcohols is preferably at least one of methanol, ethanol, n-propanol, isopropanol, n-butanol, sec-butanol, tert-butanol, iso-butanol and n-pentanol.
In some preferred embodiments of the invention, the soluble silicate is added to the dispersant-containing solution after dissolving in a solvent, preferably water, to form a silicate solution; and/or soluble aluminum salt is dissolved in a solvent, preferably water, to form an aluminum salt solution, and then the aluminum salt solution is added to the mixed solution.
According to the invention, a soluble silicate is dissolved in a solvent, preferably water, at a temperature of 20 ℃ to 35 ℃, preferably at room temperature, to form a silicate solution; and/or dissolving a soluble aluminium salt in a solvent, preferably water, at a temperature of from 40 ℃ to 80 ℃, preferably from 50 ℃ to 65 ℃, to form an aluminium salt solution, more preferably incubating the formed aluminium salt solution for from 0.5h to 2h.
According to the invention, the dissolution operation carried out in the above-mentioned temperature range is advantageous for the adequate dissolution of the soluble silicate and the soluble aluminium salt and for the stability during subsequent use.
In some preferred embodiments of the invention, the concentration of silicate in the silicate solution is 10% to 45%, preferably 25% to 30%; and/or the concentration of the aluminum salt in the aluminum salt solution is 5-35%, preferably 15-20%.
According to the present invention, when the concentration of the silicate and the concentration of the aluminum salt are within the above-specified ranges, it is advantageous to obtain aluminum silicate having a good dispersibility and a small particle size.
In another aspect, the present invention provides an aluminum silicate produced according to the above-described production method, which is free of fibrous structures, preferably having a spherical or spheroidal structure.
In some preferred embodiments of the invention, the aluminium silicate has a particle size of 500nm to 6000nm, preferably 500nm to 1500nm.
In the present invention, unless otherwise specified, "water" means deionized water, and room temperature means 25 ℃.
The preparation method of the aluminum silicate provided by the invention has the advantages of simple preparation process, economic and environment-friendly process, and the prepared aluminum silicate has the particle size of below 5000nm and most of the aluminum silicate is in a spherical or spheroidal structure.
Drawings
FIG. 1 shows an SEM picture of the aluminum silicate obtained in example 1.
FIG. 2 shows an SEM picture of the aluminum silicate obtained in example 2.
Detailed Description
The present invention will be described in detail below with reference to examples, but the scope of the present invention is not limited to the following description.
The aluminum silicates prepared in examples 1 to 10 and comparative example 1 were tested and analyzed in the following manner.
Particle size of aluminum silicate: the resulting aluminum silicate suspension was tested using a laser particle sizer to determine the particle size of the aluminum silicate.
Scanning Electron Microscope (SEM) testing of aluminum silicate: and naturally air-drying the aluminum silicate suspension drop on a copper sheet, and then carrying out SEM observation to obtain an SEM picture.
The apparatus used in the following examples 1-10, comparative example 1 includes but is not limited to:
electric mixer, shanghai sele instruments ltd, model: HD2010W;
laser particle sizer, horiba, model SZ-100Z;
scanning electron microscope, nippon electronics Co., ltd., model JSM-6700F.
The reagents used in the following examples 1-10, comparative example 1 include, but are not limited to:
sodium silicate nonahydrate, shanghai Michelin Biochemical technology, inc.;
aluminum sulfate octadecahydrate, shanghai Michelin Biochemical technology, inc.;
sodium polyacrylate, shanghai Michelin Biochemical technology, inc.
Example 1
Preparing 80g of sodium polyacrylate water solution (the mass fraction of sodium polyacrylate is 6%), and placing the sodium polyacrylate water solution into a three-neck flask to serve as a bottom material;
dissolving 39.1g of sodium silicate nonahydrate in 20g of deionized water at room temperature to obtain 59.1g of sodium silicate solution (the mass fraction of the sodium silicate is 28%);
under the condition of water bath at 60 ℃, 19.46g of aluminum sulfate octadecahydrate is dissolved in 40g of deionized water and is kept warm for 1 hour to prepare 59.46g of aluminum sulfate solution (the mass fraction of the aluminum sulfate is 16.8%);
then under the condition of stirring (the rotating speed of a high-speed stirring paddle is 1000 rpm), dropwise adding the prepared sodium silicate solution into the sodium polyacrylate aqueous solution at the speed of 0.66g/min by using a peristaltic pump to prepare suspension containing sodium silicate and sodium polyacrylate; then, dropwise adding the prepared aluminum sulfate solution into the prepared suspension at the speed of 0.99g/min by using a peristaltic pump, and continuously stirring for 12 hours after the dropwise adding is finished to prepare the aluminum sulfate-containing suspension (wherein the mass ratio of the sodium silicate nonahydrate to the sodium polyacrylate is 8:1, and the mass ratio of the sodium silicate nonahydrate to the aluminum sulfate octadecahydrate is 2:1);
then washing the prepared aluminum silicate suspension by using methanol, and drying at 70 ℃ for 12h to obtain the aluminum silicate.
The particle size of the prepared aluminum silicate is 1000nm-1100nm through testing. The suspension containing aluminium silicate obtained was left to stand at room temperature and after 28 days a separation of 5mL of supernatant was observed, indicating that the dispersibility of aluminium silicate was good and the suspension of aluminium silicate was relatively stable.
Example 2
Preparing 240g of sodium polyacrylate aqueous solution (the mass fraction of the sodium polyacrylate is 13%), and placing the sodium polyacrylate aqueous solution in a three-neck flask as a bottom material;
117.31g sodium silicate nonahydrate is dissolved in 60g deionized water at room temperature to prepare 177.31g sodium silicate solution (the mass fraction of the sodium silicate is 28%);
under the water bath condition of 65 ℃, 58.38g of aluminum sulfate octadecahydrate is dissolved in 120g of deionized water and is kept warm for 1 hour to prepare 178.38 aluminum sulfate solution (the mass fraction of the aluminum sulfate is 16.8 percent);
then under the condition of stirring (the rotating speed of a high-speed stirring paddle is 1000 rpm), dropwise adding the prepared sodium silicate solution into the sodium polyacrylate aqueous solution at the speed of 1.97g/min by using a peristaltic pump, after dropwise adding for 0.5h, dropwise adding the prepared aluminum sulfate solution at the speed of 2.97g/min by using the peristaltic pump while dropwise adding the sodium silicate solution, and continuously stirring for 12h after dropwise adding is completed to prepare an aluminum silicate-containing suspension (wherein the mass ratio of sodium nonahydrate to sodium polyacrylate is 3.75; the mass ratio of sodium nonahydrate to aluminum octadecahydrate is 2:1);
then washing the prepared aluminum silicate suspension by using deionized water, and drying for 18 hours at 105 ℃ to obtain the aluminum silicate.
The particle size of the prepared aluminum silicate is 900nm-1000nm through testing. The prepared suspension containing the aluminum silicate is kept still at room temperature, and no phenomenon of supernatant separation is observed after 28 days, which shows that the aluminum silicate has good dispersibility and is stable.
Example 3
An aluminum silicate was prepared in the same manner as in example 2 except that the mass fraction of sodium polyacrylate was 20%, and the prepared aluminum silicate was tested to have a particle size of 2400nm. The suspension containing aluminum silicate obtained was allowed to stand at room temperature, and after 28 days, 3mL of supernatant was observed, indicating that the aluminum silicate was dispersed well and the suspension of aluminum silicate was stable.
Example 4
An aluminum silicate was prepared in the same manner as in example 2 except that the mass fraction of sodium polyacrylate was 25%, and the prepared aluminum silicate was tested to have a particle size of 3000nm. The suspension containing aluminium silicate obtained was left to stand at room temperature and after 28 days 1mL of supernatant was observed, indicating that the dispersibility of aluminium silicate was good and the suspension of aluminium silicate was relatively stable.
Example 5
An aluminum silicate was prepared in the same manner as in example 1 except that the mass fraction of sodium polyacrylate was 30%, and the prepared aluminum silicate was tested to have a particle size of 5000nm. The suspension containing aluminum silicate obtained was allowed to stand at room temperature, and after 28 days, 1mL of supernatant was observed, indicating that the dispersibility of aluminum silicate was good and the suspension of aluminum silicate was stable.
Example 6
Aluminum silicate was prepared in the same manner as in example 2 except that the mass ratio of sodium silicate nonahydrate to sodium polyacrylate was 4:1, and the prepared suspension was tested to generate more aluminum hydroxide precipitate, affecting the final product quality.
Example 7
Aluminum silicate was prepared in the same manner as in example 2 except that the mass ratio of sodium silicate nonahydrate to aluminum sulfate octadecahydrate was 1:1, and the prepared suspension was tested to generate more aluminum hydroxide precipitate, affecting the final product quality.
Example 8
An aluminum silicate was prepared in the same manner as in example 1 except that "an aqueous 6% by mass ammonium polyacrylate solution" was used instead of the aqueous 6% by mass sodium polyacrylate solution in example 1, and it was tested that the particle size of the aluminum silicate obtained was 1000nm. The suspension containing aluminum silicate obtained was allowed to stand at room temperature, and 7mL of supernatant was observed after 28 days, indicating that the dispersibility of aluminum silicate was good and the suspension of aluminum silicate was stable.
Example 9
An aluminum silicate was prepared in the same manner as in example 1, except that a "28% by mass potassium sulfate solution" was used instead of a "28% by mass sodium silicate solution", and it was tested that the aluminum silicate was prepared to have a particle size of 1100 to 1200nm. The suspension containing aluminum silicate obtained was allowed to stand at room temperature, and after 28 days, 4mL of supernatant was observed, indicating that the aluminum silicate was dispersed well and the suspension of aluminum silicate was stable.
Example 10
An aluminum silicate was prepared in the same manner as in example 1, except that "16.8% by mass of aluminum chloride was used" instead of "16.8% by mass of an aluminum sulfate solution", and it was tested that the aluminum silicate was prepared to have a particle diameter of 1900 to 2000nm. The suspension containing aluminium silicate obtained was left to stand at room temperature and after 28 days a precipitation of 3mL of supernatant was observed, indicating that the dispersibility of aluminium silicate was good and the suspension of aluminium silicate was relatively stable. Comparative example 1
Dissolving 39.1g of sodium silicate nonahydrate in 20g of deionized water at room temperature to obtain 59.1g of sodium silicate solution (the mass fraction of the sodium silicate is 28%);
under the condition of water bath at 60 ℃, 19.46g of aluminum sulfate octadecahydrate is dissolved in 40g of deionized water and is kept warm for 1 hour to prepare 59.46g of aluminum sulfate solution (the mass fraction of the aluminum sulfate is 16.8%);
then under the condition of stirring (the rotating speed of a high-speed stirring paddle is 1000 rpm), dropwise adding the prepared sodium silicate solution into 80g of aqueous solution at the speed of 0.66g/min by using a peristaltic pump, and continuously stirring for 0.5h after dropwise adding is finished to prepare aqueous solution containing sodium silicate; then, dropwise adding the prepared aluminum sulfate solution into the prepared suspension at the speed of 0.99g/min by using a peristaltic pump, and continuously stirring for 12 hours after the dropwise adding is finished to prepare an aqueous solution containing aluminum sulfate precipitates;
then washing the prepared water solution containing the aluminum silicate precipitate by using methanol, and drying at 70 ℃ for 12h to prepare the aluminum silicate.
The aluminium silicate produced was tested to have a particle size of 1700nm. In addition, since no dispersant was used in this comparative example, the reaction would produce an aluminum silicate precipitate rather than forming an aluminum silicate suspension.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (6)
1. A preparation method of aluminum silicate comprises the following steps:
1) Adding soluble silicate into a solution containing a dispersing agent to form a mixed solution;
2) Adding soluble aluminum salt into the obtained mixed solution, so that the soluble aluminum salt reacts with the soluble silicate to generate aluminum silicate,
in the step 1), the dispersing agent is sodium polyacrylate, and the concentration of the dispersing agent in the solution containing the dispersing agent is 13%;
the soluble silicate is sodium silicate nonahydrate;
the soluble aluminum salt is aluminum sulfate octadecahydrate;
the mass ratio of the soluble silicate to the dispersant is 3.75;
the mass ratio of the soluble silicate to the soluble aluminum salt is 2:1.
2. The production method according to claim 1, wherein in step 1), the addition is in the form of dropwise addition; and/or in step 2), the addition is in the form of dropwise addition.
3. The production method according to claim 1 or 2, characterized in that, in step 1), soluble silicate is dissolved in a solvent to form a silicate solution, and then added to the dispersant-containing solution; and/or in the step 2), soluble aluminum salt is dissolved in the solvent to form an aluminum salt solution, and then the aluminum salt solution is added into the mixed solution.
4. The method according to claim 3, wherein in step 1), the solvent is water; and/or in step 2), the solvent is water.
5. The method according to claim 3, wherein the silicate solution has a silicate concentration of 28%; and/or the concentration of the aluminum salt in the aluminum salt solution is 16.8%.
6. Aluminum silicate produced by the production method according to any one of claims 1 to 5, characterized in that it contains no fibrous structures, has a spherical or spheroidal structure, and has a particle size of 900nm to 1000nm.
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