CN112110463A - Al (OH) based on aluminum-gallium-based alloy3Powder preparation method - Google Patents
Al (OH) based on aluminum-gallium-based alloy3Powder preparation method Download PDFInfo
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Abstract
The invention discloses Al (OH) based on aluminum-gallium-based alloy3A powder preparation method comprising: (1) mixing Al-Ga base alloy with AlCl3The solution is subjected to hydrolysis hydrogen production reaction, wherein the AlCl3AlCl in solution3The concentration of (A) is not more than 1 mol/L; (2) carrying out solid-liquid separation on the solution obtained after the reaction in the step (1); (3) and (3) heating the reaction liquid obtained after solid-liquid separation in the step (2) to 70-90 ℃, adding a weak base solution, mixing and stirring until a precipitate is not generated, aging, carrying out solid-liquid separation, and drying to obtain the aluminum hydroxide powder. The invention realizes the high-efficiency separation of unreacted alloy components and powder in the alloy by preparing the reaction liquid, improves the purity of the prepared aluminum hydroxide powder and solves the problems of raw materials, operation equipment and operation method of the aluminum hydroxide powder.
Description
Technical Field
The invention belongs to the field of hydrogen production by hydrolysis of aluminum-gallium-based alloy, and particularly relates to Al (OH) based on aluminum-gallium-based alloy3A method for preparing powder.
Background
The mass energy density and the volume energy density of the metal aluminum are high, namely 31.1MJ/kg and 83.8MJ/L, respectively, but the dense oxide film on the surface of the metal aluminum seriously hinders the energy conversion rate of the metal aluminum in the aqueous solution. The metal aluminum can be effectively activated by doping low-melting-point metal components Ga, In, Sn and the like In the metal aluminum, and the reaction activity of the aluminum In an aqueous solution is improved. Researches show that In the Al-Ga-In-Sn quaternary alloy, a low-melting-point metal component mainly serves as an efficient activation component and mainly serves as an alloy catalyst component, and exists In the alloy In the form of Al (Ga) solid solution, an alloy compound consisting of In and Sn and the like; meanwhile, the low-melting-point component in the aluminum alloy does not participate in the actual aluminum water reaction, so that the corresponding hydrolysis products are mainly aluminum ion hydrate and unreacted low-melting-point metal components.
Al(OH)3The powder is white powder, is almost insoluble in water, has a relative density of 2.42 and a Mohs hardness of 3.0; no toxicity, good stability and no generation of toxic gas at high temperature; can effectively reduce the smoke amount and the like when the plastic is burnt. At present, the aluminum hydroxide used as a flame retardant in the domestic and foreign markets is mainly alpha-alumina trihydrate (chemical formula: a-Al)2O3·3H2O), the loss of about 34.6% of its weight due to loss of water when heated to 320 ℃, while absorbing a large amount of heat (about 1967.2kJ/kg), which is Al (OH)3The powder has a main reason for its flame retardant action. In addition, Al (OH)3The powder flame retardant effect is also dependent on the dilution, coating and carbonization that occurs at high temperatures. Therefore Al (OH)3Becomes an inorganic flame retardant additive with the most application value and application prospect, and is widely applied to thermosetting plastics, thermoplastic plastics, synthetic rubber, coating, building materials and other industries. Al (OH)3Cheap, widely available and commonly used Al (OH)3The industrial preparation method of the powder is mainly a Bayer sintering combination method.
Bayer sintering combination method for producing Al (OH)3The Bayer process and the soda lime sintering process are effectively combined, the Bayer process is mainly used, the soda lime sintering process is used as an auxiliary process, and the advantages of the two preparation methods are fully exerted.
The Bayer process is to dissolve alumina in bauxite by heating sodium hydroxide solution to obtain sodium aluminate solution. Separating the residue (red mud), reducing the temperature, adding aluminum hydroxide as a growth seed crystal, and stirring for a long time to decompose the sodium aluminate and separate out the aluminum hydroxide. The method has simple process operation, low investment cost and low energy consumption, but the economic effect of the production mainly depends on the quality of the bauxite. At present, the bayer process is hindered in the field of aluminum hydroxide production because of the gradual decrease in high-grade gibbsite type bauxite resources.
The soda lime sintering method is to mix bauxite, sodium carbonate and lime according to a certain proportion and sinter them in a rotary kiln to obtain clinker (mainly comprising sodium aluminate, sodium ferrite, calcium orthosilicate and sodium titanate). And dissolving out the sodium aluminate in the clinker by using a dilute alkali solution. The sodium aluminate solution obtained by dissolution is purified by a special desilication process. Introducing CO2Introducing gas into the refined sodium aluminate solution, and stirring with the added aluminum hydroxide seed crystal to obtain a mother liquor mainly containing aluminum hydroxide precipitate and sodium carbonate. The method can be used for treating low-grade ores which cannot be economically treated in the Bayer process, and has better comprehensive utilization of the original ores.
Al (OH) can be prepared by hydrolyzing aluminum-rich alloy3The method for preparing the powder is relatively simple and convenient, the powder has small particle size and uniform distribution, and the flame retardant property of the powder can be directly influenced by the reduction of the powder particles, so that the surface area of the corresponding particles is increased due to the smaller particle size, the water vapor pressure on the surfaces of the particles is promoted to be increased, and the improvement of the flame retardant property is facilitated. The hydrolytic activity of the alloyed aluminum alloy is improved, so that Al (OH)3The powder can be prepared in a simple environment with high efficiency and large amount, but Al (OH)3The activated components of Ga, In, Sn and the like doped In the powder and not participating In the hydrolysis reaction reduce the purity of the powder and the recovery rate of the powder. Meanwhile, the cost of the raw materials is also rich in aluminum alloy Al (OH)3One of the limiting factors in the field of powder preparation.
Disclosure of Invention
The invention aims to provide Al (OH) based on aluminum-gallium-based alloy3The powder preparation method has simple impurity separation and is beneficial to improving the purity of the prepared aluminum hydroxide powder.
In order to achieve the purpose, the invention adopts the following technical scheme:
based on aluminium-gallium base alloyAl(OH)3A method of preparing a powder comprising the steps of:
(1) mixing Al-Ga base alloy with AlCl3The solution is subjected to hydrolysis hydrogen production reaction, wherein the AlCl3AlCl in solution3The concentration of (A) is not more than 1 mol/L;
(2) carrying out solid-liquid separation on the solution obtained after the reaction in the step (1);
(3) and (3) heating the reaction liquid obtained after solid-liquid separation in the step (2) to 70-90 ℃, adding a weak base solution, mixing and stirring until a precipitate is not generated, aging, carrying out solid-liquid separation, and drying to obtain the aluminum hydroxide powder.
In the present invention, the aluminum-gallium-based alloys that can be hydrolyzed to produce hydrogen are those known in the art, in which aluminum can be directly hydrolyzed with water to produce hydrogen, and are well known in the art. In one embodiment, the aluminum-gallium-based alloy is an Al-Ga-In-Sn alloy commonly used In the field of hydrogen production by hydrolysis, and optionally, the aluminum-gallium-based alloy further contains an X metal component selected from one or more of metals bismuth, zinc, iron, copper, magnesium and titanium to replace part of gallium, indium and tin, thereby reducing the amount of noble metal, wherein the content of the substitute metal X is not more than 10 wt%, preferably, the content of the X metal component is not more than 8 wt%, and further preferably, not more than 6 wt%, such as 0.1 wt%, 0.5 wt%, 1 wt% or 4 wt%. The aluminum gallium based alloy may include 80 wt% to 94 wt%, such as 82 wt%, 85 wt%, 88 wt%, 90 wt% or 92 wt% aluminum, 2 wt% to 5 wt%, such as 3 wt% or 4 wt% gallium, 3 wt% to 16 wt%, such as 5 wt%, 8 wt%, 10 wt%, 12 wt% or 15 wt% indium and tin, wherein the sum of the contents of aluminum, gallium, indium and tin is not less than 90 wt%, such as 95 wt% or 98 wt%.
Methods for preparing the above-described aluminum-gallium-based alloys are well known in the art and, in one embodiment, may be prepared by:
(a) weighing the metals according to the proportion, putting the weighed metals into a furnace protected by nitrogen, heating at 700-1000 ℃, such as 800 ℃, and keeping the temperature for 0.5-2h, such as 1 h. Preferably, the individual metals used have a purity of > 99 wt.%, for example 99.9 wt.%.
(b) And stirring the sample after heat preservation, pouring the sample into a mold, and cooling, preferably naturally cooling in air to obtain the alloy. And packaging the cooled alloy, and storing for a long time.
In the invention, researches show that the aluminum-gallium-based alloy is in the AlCl of the invention3In the hydrolysis in solution, the aluminium hydroxide obtained after hydrolysis of aluminium does not form a precipitate, but rather is Al (OH)3Is in the form of colloid, preferably, in the step (1), the AlCl is present3AlCl in solution3The concentration of (b) is 0.1 to 1mol/L, such as 0.2mol/L, 0.4mol/L, 0.6 or 0.8mol/L, etc., and in one embodiment may be 0.1 to 0.5mol/L, and in one embodiment may be 0.5 to 1 mol/L.
According to the method of the present invention, preferably, when the aluminum-gallium-based alloy and the reaction solution are subjected to hydrolysis hydrogen production reaction, the liquid-solid ratio (the ratio of the volume of the liquid phase to the mass of the solid-phase alloy) is not less than 15L/Kg, preferably 18 to 25L/Kg, such as 20L/Kg, 22L/Kg or 24L/Kg, and the reaction temperature is 20 to 60 ℃, such as 25 ℃, 35 ℃, 40 ℃, 45 ℃ or 55 ℃, preferably 30 to 50 ℃.
In the step (2) of the present invention, the reaction solution is subjected to solid-liquid separation to obtain a clear liquid phase or a reaction solution, thereby separating a by-product (residue) of unreacted metal, and aluminum hydroxide exists in the separated liquid phase. According to the method of the present invention, preferably, in the step (2), solid-liquid separation is performed by a centrifugal method, for example, solid-liquid separation or cyclone separation using a high-speed centrifuge.
In the step (3), the reaction solution obtained after solid-liquid separation is heated to 70-90 ℃, such as 75 ℃, 80 ℃ or 85 ℃, and added with alkali solution to be mixed and stirred until no precipitate is generated, and the aluminum hydroxide powder is obtained through aging, solid-liquid separation and drying. Preferably, the aging temperature before solid-liquid separation is 120-160 ℃, such as 130, 140 or 150 ℃ (such as closed aging), and the aging time is 2-4 hours, such as 3 hours, so as to stabilize the property and state of the precipitate obtained by conversion. The alkali solution can be ammonia water, sodium hydroxide or potassium hydroxide solution, and is preferably weak alkali solution. The amount of the weak base added can be judged according to the pH value of the reaction solution until the pH value of the reaction solution reaches 8-9.
In one embodiment of the present invention, the method further comprises step (4): collecting the separated reaction residues, and washing and drying the collected residues to obtain a metal byproduct; preferably, the number of washes in the washing is at least one, and the washing liquid used for washing is diluted hydrochloric acid at least once, for example, diluted hydrochloric acid having a concentration of 0.1 to 1mol/L, such as 0.2mol/L, 0.4mol/L or 0.6mol/L, in an amount of not more than 5 times, such as 1 to 4 times, for example 2 or 3 times, the volume of the solid phase to be washed.
In the invention, due to the action of the reaction liquid, the aluminum in the alloy can not form a precipitate after hydrolysis, so that the solid phase is a metal or an intermetallic compound which does not participate in the hydrolysis reaction in the aluminum-gallium-based alloy, thereby being convenient for recycling.
Compared with the prior art, the invention has the following advantages:
the invention utilizes aluminum-based alloy and AlCl3The reaction liquid is reacted to produce hydrogen, simultaneously, the unreacted alloy components and powder in the alloy are efficiently separated by preparing the reaction liquid, the purity of the prepared aluminum hydroxide powder is improved, and the problems of the aluminum hydroxide powder to the raw materials, the operation equipment and the operation method can be solved because the raw materials are simply introduced in the reaction. In AlCl3In the solution, the final energy conversion of the Al-Ga-In-Sn alloy is still kept to be approximately 100 percent, and the reaction liquid after the reaction is In a clear and transparent state, so that the aluminum hydrate ions after the reaction are efficiently separated from the solid sediments which do not participate In the reaction In the alloy, and the purity of the aluminum hydroxide powder obtained by colloid conversion is improved. The preparation method is simple and quick to operate, the requirement on a production device is low, the production cost is reduced, the industrial production efficiency of the aluminum hydroxide powder is further improved, and the mass industrial production process of the aluminum hydroxide is promoted.
Drawings
FIG. 1 is an XRD pattern of the Al-Ga-In-Sn alloy of example 1;
FIG. 2 is a graph showing the visible light transmittance of the solution after solid-liquid separation in each example.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
Unless otherwise specified, the following reagents were used analytically pure, with a metal feedstock purity of greater than 99.9 wt.%.
Examples 1 to 4
And preparing an alloy sample according to the proportion, introducing nitrogen as protective gas In the preparation process, preserving the heat for 1h at 800 ℃, and casting to obtain the Al-Ga-In-Sn quaternary alloy. Prepared Al-Ga-In-Sn quaternary alloy and AlCl3The aqueous solution is hydrolyzed to prepare hydrogen, which comprises the following specific steps:
1) reacting the prepared Al-Ga-In-Sn quaternary alloy with AlCl3 solutions with different concentrations to prepare aluminum hydroxide powder, wherein the concentrations of AlCl3 are 0.1mol/L, 0.2mol/L, 0.3mol/L and 0.4mol/L respectively;
2) placing the reacted reaction system in a high-speed centrifuge for high-speed centrifugation for 5min to obtain a clear reaction solution without impurities, and completing a corresponding visible light transmittance test on the reaction solution as shown in figure 2;
3) adding light beams on the side surface of the reaction solution, observing that a bright light path channel is generated In the solution, and indicating that the reaction solution obtained by the Al-Ga-In-Sn quaternary alloy In AlCl3 is mainly Al (OH)3 colloid;
4) taking 200mL of the supernatant after reaction, heating to 80 ℃, mixing with 80mL of concentrated ammonia water, stirring, converting Al (OH)3 colloid into Al (OH)3 precipitate, and stopping dropwise adding the concentrated ammonia water until the precipitate is not generated any more;
5) aging the obtained Al (OH)3 precipitate at 150 ℃ for 3h, and separating the precipitate by suction filtration;
6) the above precipitates were dried at 140 c for 3 hours to obtain the final aluminum hydroxide powder, and the finally prepared aluminum hydroxide powder was analyzed for particle size, yield and purity as shown in table 1-2.
The specific mixture ratio of the alloy of the embodiment 1 and the alloy of the embodiment 2 is 80 wt% of aluminum, 5 wt% of gallium, 15 wt% of indium and tin, wherein the mass ratio of indium to tin is 3: 1; the alloy of examples 3 and 4 was specified as 90 wt% aluminum, 2.5 wt% gallium, 7.5 wt% indium and tin, with the mass ratio of indium to tin being 3: 1.
TABLE 1 Al (OH) prepared in the reaction solution at different concentrations3Purity (wt%) and particle size (unit: mum) statistics of the powder
TABLE 2 Al (OH) of the Rich aluminum alloy System3Statistics of powder yield
| AlCl3Concentration of solution (mol/L) | 0.1 | 0.2 | 0.3 | 0.4 |
| Yield (%) | 75.33 | 90.67 | 99.98 | 94.25 |
Claims (9)
1. Al (OH) based on aluminum-gallium-based alloy3A method of preparing a powder comprising the steps of:
(1) mixing Al-Ga base alloy with AlCl3The solution is subjected to hydrolysis hydrogen production reaction, wherein the AlCl3AlCl in solution3The concentration of (A) is not more than 1 mol/L;
(2) carrying out solid-liquid separation on the solution obtained after the reaction in the step (1);
(3) and (3) heating the reaction liquid obtained after solid-liquid separation in the step (2) to 70-90 ℃, adding a weak base solution, mixing and stirring until a precipitate is not generated, aging, carrying out solid-liquid separation, and drying to obtain the aluminum hydroxide powder.
2. The method of claim 1, wherein in step (1), the AlCl is present3AlCl in solution3The concentration of (b) is 0.1 to 1 mol/L.
3. The method according to claim 1 or 2, wherein in the step (3), the aging temperature is 120 to 160 ℃ and the aging time is 2 to 4 hours; preferably, the drying temperature is 110-160 ℃.
4. The method according to any one of claims 1 to 3, wherein in the step (2), solid-liquid separation is performed by centrifugation.
5. The method according to any one of claims 1-4, characterized in that the method further comprises step (4): and collecting the separated reaction residues, and washing and drying the collected reaction residues to obtain the metal by-product.
6. The method according to claim 5, wherein in the step (3), the number of washing times in the washing is at least one, and the washing liquid used for the washing is diluted hydrochloric acid at least once.
7. The method according to any one of claims 1 to 6, wherein the aluminum gallium based alloy is an Al-Ga-In-Sn alloy; optionally, the aluminum-gallium-based alloy further comprises an X metal component, wherein the X metal component is one or more selected from metal bismuth, zinc, iron, copper, magnesium and titanium; wherein the sum of the contents of aluminum, gallium, indium and tin is not less than 90 wt%, preferably not less than 95 wt%, and more preferably not less than 98 wt%.
8. The method of claim 7, wherein the aluminum gallium based alloy comprises 80 wt% to 94 wt% aluminum, 2 wt% to 5 wt% gallium, 3 wt% to 16 wt% indium, and tin.
9. The method according to any one of claims 1 to 8, wherein the liquid-solid ratio of the aluminum-gallium-based alloy and the reaction solution is not less than 15L/Kg, preferably 18 to 25L/Kg, and the reaction temperature is 20 to 60 ℃, preferably 30 to 50 ℃ when the aluminum-gallium-based alloy and the reaction solution are subjected to hydrolysis hydrogen production.
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