CN109879262B - Preparation method of powdery high-purity aluminum metaphosphate suitable for optical glass - Google Patents
Preparation method of powdery high-purity aluminum metaphosphate suitable for optical glass Download PDFInfo
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Abstract
The invention discloses a method for preparing powdery high-purity aluminum metaphosphate suitable for optical glass, which comprises the steps of utilizing soluble aluminum salt, purifying, preparing high-purity aluminum phosphate, aluminum hydrogen phosphate or aluminum hydroxide, washing for many times to remove impurities, centrifugally drying when the conductivity of supernatant is less than or equal to 50 mu s/cm, reacting with high-purity phosphoric acid to enable P in generated aluminum dihydrogen phosphate solution2O5/Al2O3The mass ratio of the aluminum metaphosphate to the solution is 4.10-4.30, the solution is sprayed and dried, then the solution is placed in a microwave oven for reaction, a crude product of the aluminum metaphosphate is prepared, a ceramic rod is used for crushing and stirring the aluminum metaphosphate uniformly, powder is obtained, and the powder is burned by a muffle furnace to obtain a finished product. The invention has the advantages of high reaction speed, no sintering of the product with a roasting vessel, easy taking out and crushing of the product, short preparation time and high speed. The product has stable quality, uniform granularity, bright white color, high purity, the content of more than or equal to 99 percent, low content of non-ferrous metal ions, less than or equal to 2ppm of iron ions, less than 1ppm of Co, Ni and Cu, and high one-time yield and qualification rate. Is suitable for preparing products such as optical glass, special glass and the like.
Description
The technical field is as follows:
the invention belongs to the technical field of chemical engineering, and relates to a preparation method of inorganic material powder high-purity aluminum metaphosphate.
Background art:
in recent years, products such as high-purity phosphate, special phosphate, functional phosphate and the like are further popularized and applied in the aspects of advanced science and technology, national defense industry and the like. In addition, phosphate has been widely developed and applied in other fields, and a series of novel phosphate materials, such as phosphate electronic and electrical materials, phosphate optical materials, phosphate solar cell materials, phosphate sensing element materials, artificial biological materials and the like, appear. At present, the method is closely related to a plurality of scientific fields, and more related departments become an industry with important functions in national economy.
Metaphosphate is the most stable component of dibasic phosphate, and is the basic raw material for producing phosphate glass. High-purity metaphosphate is an important raw material of laser glass in a high-power laser because of excellent light transmission performance. Among the different phosphates used according to different uses, aluminum metaphosphate is most used. For example, aluminum metaphosphate has better moisture resistance and lower refractive index than other metaphosphates in the fluorophosphate glass, and has larger Abbe number, thereby leading to lower ultraviolet partial dispersion of the glass, high chemical stability and mechanical strength, and higher chemical stability by 3 orders of magnitude than the zirconium fluoride-based glass.
Generally, when the phosphate is used as a raw material for optical glass, the content of non-ferrous metal elements such as Co, Ni, Cu, Fe and the like in the phosphate exceeds 5ppm, and the degree of coloration of the obtained optical lens is drastically increased. In particular, iron is colored to a higher degree than other non-ferrous metallic elements when compared with the same concentration, and thus it is more effective to reduce the concentration of iron. From this viewpoint, the concentration of iron is preferably 5ppm or less, and particularly preferably 2ppm or less. Therefore, high purity aluminum metaphosphate for optical glass is required, and strict control and detection of process parameters during production are required.
The preparation of high-purity aluminum metaphosphate is generally carried out by high-temperature roasting of phosphoric acid raw material and aluminum compound or aluminum phosphate compound. However, since it is produced in a consolidated state, the hardness of the particles is high, the operability is poor, time and labor are wasted, and further, a process such as pulverization is required, which increases the possibility and risk of mixing of unknown impurities. And the longer the pulverization is, the larger the content of impurities will be. To prevent sintering and consolidation of the product, the literature [ Khicmichelshaya promyslenost (Moscow, Russian Federation)1982, 10, 595-7]A method of heating a reaction solution of aluminum dihydrogen phosphate produced by reacting aluminum hydroxide with phosphoric acid at a temperature of 700 ℃ to 750 ℃ in a spray dryer, but the nozzle inevitably contains impurities. Although high purity aluminum metaphosphate can be obtained as described in Japanese patent laid-open No. 2003-63811However, in the preferable reaction employed for preventing the product from being solidified, since a solid phase reaction in which the moisture is reduced to the maximum is used, there are some cases in which the reaction is difficult to complete, the reaction is not uniform, and the molar ratio (P) is not uniform205/A1203) The defect of difficult control. In addition, there is no specific description about the content of impurities. Japanese patent No. 3865604 discloses a method of mixing and baking aluminum metaphosphate with raw material powder. However, the amount of the mixed aluminum metaphosphate is 50 to 70% of the total amount of the baked material, and in the second reaction, the amount of newly produced aluminum metaphosphate is small, and the reaction efficiency is low. In addition, the mixed aluminum metaphosphate inevitably solidifies in the firing vessel at the first time during the production, and is likely to be contaminated during the pulverization. In the same manner as in japanese patent No. 3865604, japanese patent No. 3802916, which is a method for preventing the solidification of a product, is a method for adding a viscous liquid of the first step to a calcination vessel in a state where aluminum metaphosphate powder is spread, and calcining the viscous liquid obtained by reacting phosphoric acid with an aluminum compound, as in patent No. cn200480006982. The amount of the aluminum metaphosphate coated is 40-60% of the total amount of the roasted substances, and the efficiency of the method is low. Further, in this method, the formed aluminum metaphosphate is massive, which cannot completely prevent the solidification, and the degree of solidification increases as the scale grows, and this method requires pulverization inevitably, and the inclusion of impurities due to the material of the pulverizer is inevitable. The use of the hygroscopic quenching powder of the phosphoric acid in an excess amount in Japanese laid-open patent publication No. 2009-67608 can prevent the solidification, but the particles are large and non-uniform, and the subsequent washing operation is complicated due to the excess amount of phosphoric acid, and impurities introduced into the raw material cannot be removed. In patent CN20171072959.1, an aluminum source is dissolved in an alcohol solvent i, a phosphorus source is dissolved in an alcohol solvent ii, a precursor is prepared by a sol-gel method, and the precursor is obtained by high-temperature polymerization. However, P is not easily controlled by this method2O5With Al2O3The prepared intermediate is colloid and is easy to absorb impurities, and the solvent is organic solvent, so that the cost is high, the environment is not protected, the preparation temperature is high, otherwise, the solvent is leftThe decomposition of organic matters on the intermediate is not thorough, namely the product quality is influenced, the product appearance is influenced, and the product color is darker. Literature [ Wanying, preparation of high purity aluminum metaphosphate, university of Master in China, Master's treatise, P14-19]The high-purity aluminum metaphosphate is prepared by taking ammonium dihydrogen phosphate and aluminum hydroxide as raw materials, the reaction speed is slow, ammonia gas is generated during ignition, the equipment and the environment are not friendly, and the operation of operators is not facilitated. Although microwave is used in one experiment in the experimental process, the power is too low, the time is too long, firstly, the reaction is agglomerated seriously, and the reaction is not easy to take out; secondly, the production efficiency is low, the reaction is easy to be incomplete, and the impurities are high. Further, equipment such as exhaust gas treatment is required, and the content of impurities cannot be reduced.
The invention content is as follows:
the present invention has been made to solve the above-mentioned problems of the prior art, and an object of the present invention is to provide a method for producing powdery high-purity aluminum metaphosphate suitable for optical glass.
The invention uses soluble aluminum salt to prepare high-purity aluminum phosphate, aluminum hydrogen phosphate or aluminum hydroxide after purification, removes impurities by washing water for many times, centrifugally dries after the conductivity of supernatant fluid of washing sediment is less than or equal to 50 mus/cm, reacts with high-purity phosphoric acid to lead P in the generated aluminum dihydrogen phosphate solution2O5/Al2O3The mass ratio of (3) to (4.10-4.30), spray drying the solution, then placing the aluminum dihydrogen phosphate ultrafine powder in a microwave oven for reaction to prepare a crude product of the aluminum metaphosphate, crushing and stirring the crude product by using a ceramic rod to obtain powder, and firing the powder by using a muffle furnace to obtain the high-purity aluminum metaphosphate powder.
The method adopts the microwave roasting method to prepare the aluminum metaphosphate, and has the advantages of high reaction speed, no sintering of the product and the roasting vessel, easy taking out and crushing of the product, short preparation time and high speed due to the fact that the reaction process is an intramolecular reaction, and overcomes the defects that the product and the roasting vessel are sintered, the material is difficult to obtain, the product is crushed by a crusher and the like in the preparation process of the conventional aluminum metaphosphate. The product prepared by the process has stable quality, uniform granularity, bright white color, high purity, the content of more than or equal to 99 percent, low content of non-ferrous metal ions, less than or equal to 2ppm of iron ions, less than 1ppm of Co, Ni and Cu, and high one-time yield and qualified rate. Is suitable for preparing products such as optical glass, special glass and the like.
A preparation method of powdery high-purity aluminum metaphosphate suitable for optical glass comprises the following steps:
(1) preparation of high purity aluminum compound precipitate: after purifying soluble aluminum salt, adding a precipitator to prepare high-purity aluminum compound precipitate;
(2) washing: boiling the aluminum compound precipitate prepared in the step (1), then preserving heat at 70-90 ℃ for sedimentation, pouring out supernatant, taking out slurry and centrifugally drying; putting the solid into an enamel pot, adding pure water, stirring to disperse, stirring to boil, keeping the temperature, settling, pouring supernatant, centrifugally drying the slurry, repeating the steps for several times until the conductivity of the supernatant is less than or equal to 100 mu s/cm, centrifugally drying the slurry, and detecting the content and impurities;
(3) dilution of phosphoric acid: preparing a phosphoric acid solution with the concentration of 20-60% by using a phosphoric acid solution with the content of more than or equal to 85%;
(4) preparation of aluminum dihydrogen phosphate solution: the phosphoric acid solution prepared in the step (3) is injected into a reaction kettle, heated to 70-80 ℃, and then completely reacted according to P contained in the final solution2O5/Al2O3Adding one or two of aluminum hydrogen phosphate, aluminum phosphate or aluminum hydroxide in a mass ratio of 4.0-4.4;
(5) removing impurities and assisting filtration by using activated carbon: when the concentration of the solution is concentrated to 30-33Be degrees, adding activated carbon into the aluminum dihydrogen phosphate solution prepared in the step (4) to adsorb impurities in the solution, thereby achieving the purpose of removing the impurities; the using amount of the active carbon is 1-5 per mill of the volume of the solution, the time is 20-30 min, and the next step is carried out after the solution is subjected to filter pressing and cleaning;
(6) p in the filtered aluminum dihydrogen phosphate solution obtained in the step (5)2O5/Al2O3The mass ratio of (A) to (B) is finely adjusted when P is in the aluminum dihydrogen phosphate solution2O5/Al2O3The mass ratio of (1) to (4.0-4.4) can be used for the next stepAnd (4) otherwise, supplementing phosphoric acid or the treated aluminum phosphate, aluminum hydrogen phosphate or aluminum hydroxide according to the metering ratio, and continuing the operation of the steps (5) and (6).
(7) Evaporation concentration or spray drying: heating by using steam, evaporating and concentrating the solution obtained in the step (6) until a large amount of foams exist in the aluminum dihydrogen phosphate solution and a little white crystals are separated out, stopping heating, taking out and placing in a plastic barrel for cooling to obtain a very viscous solution; or directly spray-drying the solution obtained in the step (6) at the air inlet temperature of 200-240 ℃ to obtain aluminum dihydrogen phosphate powder;
(8) preparing aluminum metaphosphate by microwave heating: placing the aluminum dihydrogen phosphate viscous liquid or the aluminum dihydrogen phosphate powder obtained in the step (7) into a high-temperature-resistant and microwave-resistant ceramic vessel, placing the ceramic vessel into a microwave oven for microwave heating reaction, wherein the reaction time is determined by the amount of reaction materials, the moisture contained in the reaction materials and the microwave heating power, the reaction end point is that the materials generate a multi-gap, layered, foamed and fluffy white object, the materials are instantly and rapidly heated to more than 600 ℃ in the reaction process, and after the reaction is finished, cooling and taking out the materials;
(9) crushing aluminum metaphosphate: taking out the precursor of the aluminum metaphosphate prepared by the microwave oven reaction in the step (8), and crushing by using a ceramic rod to be uniform; the content of the aluminum metaphosphate can reach 95 to 96 percent;
(10) and (3) roasting to prepare aluminum metaphosphate: putting the aluminum metaphosphate prepared in the step (9) into a muffle furnace, and roasting at 600-800 ℃; the roasting time is determined by the thickness of the material and is generally 2-4 hours;
(11) detecting and packaging: sampling and detecting the aluminum metaphosphate obtained in the step (10), obtaining a qualified finished product, and packaging according to requirements to obtain a powdery high-purity aluminum metaphosphate finished product. The prepared powder high-purity aluminum metaphosphate can be used as an optical glass raw material.
Preferably, in the above method for producing powdery high-purity aluminum metaphosphate for optical glass: the soluble aluminum salt in the step (1) is aluminum chloride, aluminum sulfate, aluminum nitrate, aluminum ammonium sulfate or aluminum potassium sulfate.
Preferably, in the above method for preparing high purity aluminum metaphosphate powder suitable for optical glass, the method comprises the steps of: in the step (1), the precipitant is selected from potassium phosphate, sodium phosphate, ammonium phosphate, potassium hydrogen phosphate, sodium hydrogen phosphate, ammonium hydrogen phosphate and ammonia water.
Preferably, in the above method for producing powdery high-purity aluminum metaphosphate for optical glass: the conductivity of the supernatant in the step (2) is less than or equal to 50 mu s/cm.
Preferably, in the above method for producing powdery high-purity aluminum metaphosphate for optical glass: and (3) selecting the phosphoric acid solution with impurity Fe less than or equal to 2ppm and content more than or equal to 85 percent.
Preferably, in the above method for preparing high purity aluminum metaphosphate powder suitable for optical glass, the method comprises the steps of: the concentration of the phosphoric acid prepared in the step (3) is 35 to 50 percent.
Preferably, in the above method for producing powdery high-purity aluminum metaphosphate for optical glass: said P in step (6)2O5/Al2O3The mass ratio of (a) to (b) is 4.1 to 4.3.
Preferably, in the above method for producing powdery high-purity aluminum metaphosphate for optical glass: in the step (8), the power of the microwave oven is preferably more than 1000W, and the reaction temperature is rapidly increased to more than 600 ℃ due to the high-fire function.
Preferably, in the above method for producing powdery high-purity aluminum metaphosphate for optical glass: in the step (10), the roasting temperature is 650-800 ℃.
Preferably, in the above method for producing powdery high-purity aluminum metaphosphate for optical glass: and (2) precipitating the high-purity aluminum hydrogen phosphate, aluminum phosphate or hydroxide prepared in the step (1), wherein the content of Fe in the detected impurity is less than or equal to 2.0ppm, and preferably the content of Fe is less than or equal to 1.0 ppm. The aluminum dihydrogen phosphate solid is prepared by preferably spray drying in the step (7), which is beneficial to the subsequent microwave heating, the operation is convenient, and impurities are not easy to introduce. In the step (8) and the step (10), the container does not introduce impurities, particularly non-ferrous metal ion impurities.
Compared with the prior art, the invention has the following beneficial effects:
the invention overcomes the problems that the product is sintered with a roasting vessel in the preparation process of the traditional aluminum metaphosphate, the material is difficult to obtain, the product needs to be crushed by a special crusher, and the like. The high-purity aluminum metaphosphate prepared by the microwave method has the advantages of high reaction speed, difficult sintering of a product and easy taking out of a roasting vessel due to the fact that the reaction process is an intramolecular reaction, short preparation time, high efficiency and high speed, and the product has stable quality, uniform granularity, basically can pass through a 80-mesh sieve, is bright and white in color and high in purity, has the content of more than or equal to 99 percent and low content of nonferrous metal ions, iron ions are less than or equal to 2ppm, nonferrous metal ions such as Co, Ni, Cu, Mn and the like are less than 1ppm, and has high one-time yield and qualified rate. The product prepared by the preparation method is suitable for preparing products such as optical glass, special glass and the like
Description of the drawings:
fig. 1 is an XRD pattern of high-purity aluminum metaphosphate prepared by microwave roasting.
The specific implementation mode is as follows:
the present invention will be further described below by way of specific examples, but in the following description, "%" and "ppm" are based on weight unless otherwise specified. The high-purity aluminum metaphosphate of the present invention contains impurity concentration of various nonferrous metal elements below 2 ppm.
The method for measuring the content of each nonferrous metal in the aluminum metaphosphate comprises the following steps: the prepared aluminum metaphosphate is dissolved in an acid solution, the test sample is prepared after clarification, the measurement sample is measured by ICP emission spectrometry, and the content of phosphorus pentoxide and the content of aluminum oxide are measured by a chemical analysis method. The XRD pattern was obtained by X-ray diffractometer scanning.
The present invention will be described in detail with reference to examples, but the scope of the present invention is not limited thereto.
Example 1:
(1) preparing high-purity aluminum phosphate precipitate: weighing 24kg of purified aluminum chloride and 20kg of diammonium phosphate, preparing 20% solutions respectively, slowly adding the aluminum chloride solution into the diammonium phosphate solution according to the stoichiometric ratio under the stirring state, and preparing aluminum phosphate precipitate.
(2) Washing: boiling the aluminum hydrogen phosphate precipitate prepared in the step (1), then preserving heat at 70-90 ℃ for sedimentation, pouring supernate (the supernate is recycled to prepare a byproduct), taking out the serous fluid, and centrifuging and drying. Putting the solid into an enamel pot, adding pure water, stirring to disperse, stirring to boil, keeping the temperature, settling, pouring the supernatant, centrifugally drying the slurry, repeating the steps for several times until the conductivity of the supernatant is less than or equal to 50 mu s/cm, centrifugally drying the slurry, and checking the content.
(3) And (3) dilution of phosphoric acid: 16.6kg of 85% phosphoric acid was weighed out to prepare 35% phosphoric acid.
(4) Preparation of aluminum dihydrogen phosphate solution: the phosphoric acid solution prepared in the step (3) is injected into a reaction kettle, heated to 70-80 ℃, and then completely reacted according to P contained in the final solution2O5/Al2O316.5kg of aluminum hydrogen phosphate is added in the mass ratio of (1) to (4.0-4.4).
(5) Removing impurities and assisting filtration by using activated carbon: when the concentration of the solution is concentrated to 32Be degrees, adding activated carbon into the aluminum dihydrogen phosphate solution prepared in the step (4) to adsorb impurities (such as organic matters) in the solution, thereby achieving the purpose of removing the impurities; the usage amount of the active carbon is 25g, the time is 30min, and the next step is carried out after the filter pressing is clear.
(6) Detecting P in the filtered aluminum dihydrogen phosphate solution in the step (5)2O5/Al2O3The mass ratio of the P-containing compound is finely adjusted when the P-containing compound is in the aluminum dihydrogen phosphate solution2O5/Al2O3The mass ratio of (3) to (2) is 4.20, and the next process can be carried out.
(7) Spray drying: and (4) directly carrying out spray drying on the solution obtained in the step (6) at the air inlet temperature of 200-240 ℃ to obtain the aluminum dihydrogen phosphate powder.
(8) Preparing aluminum metaphosphate by microwave heating: and (3) placing the aluminum dihydrogen phosphate solid powder obtained in the step (7) into a high-temperature-resistant and microwave-resistant ceramic vessel, placing the ceramic vessel into a microwave oven for microwave heating reaction, wherein the microwave heating power is 2000W, the time is 3min, the reaction end point is that the material generates a multi-gap and layered foaming white object, the material is instantly and rapidly heated to more than 600 ℃ in the reaction process, and after the reaction is finished, cooling and taking out the material.
(9) Crushing aluminum metaphosphate: and (3) taking out the aluminum metaphosphate prepared by the microwave oven reaction in the step (8), crushing the aluminum metaphosphate by using a ceramic rod, uniformly spreading the aluminum metaphosphate, enabling 95% of powder to pass through a 80-mesh sieve, enabling a small part of powder to pass through the 80-mesh sieve, and pressing the powder by using the rod again, wherein the powder can basically pass through the 80-mesh sieve. At this time, the content of aluminum metaphosphate can reach 95-96%, but a small amount of weight loss can be generated.
(10) And (3) roasting to prepare aluminum metaphosphate: and (4) putting the aluminum metaphosphate prepared in the step (9) into a muffle furnace, and roasting at 650 ℃ for 2 hours.
(11) Detection and packaging: 24.6kg of the aluminum metaphosphate sample obtained in the step (10) was sampled and detected, and the sample was numbered S1, and the yield was 95%.
Example 2:
24kg of purified aluminum chloride and 20kg of purified diammonium phosphate, 16.6kg of phosphoric acid with the content of 85 percent and the Fe content of less than or equal to 1ppm, and the rest steps are the same as the example 1 and are different from the step (7) and the step (8). Example 2 in the step (7), the aluminum dihydrogen phosphate solution is concentrated into a viscous liquid which is slightly whitish, and in the step (8), the viscous liquid is put into a high-temperature-resistant and microwave-resistant ceramic dish for microwave heating reaction, wherein the microwave power is 2000w, and the time is 5 min. Step (9), step (10) and step (11) are the same as in example 1. The sample produced in example 2 was designated as S2, and weighed 24.8kg with a yield of 96%.
Example 3:
45.3kg of purified aluminum ammonium sulfate (Fe is less than or equal to 0.1ppm) and 15kg of ammonium phosphate (Fe is less than or equal to 0.1ppm) are reacted to prepare an intermediate product, namely aluminum phosphate precipitate, and then the intermediate product is reacted with 22.5kg of phosphoric acid with 85 percent of Fe being less than or equal to 1ppm to prepare aluminum dihydrogen phosphate solution. The procedure was carried out in the same manner as in example 1 except that 24.9kg of the sample prepared in example 3 was designated by the reference numeral S3. The one-time yield is 94%, the particles are fine and uniform, the color is bright white, the Fe ion is less than 2ppm, and the Co, Ni and Cu are less than 1 ppm.
Example 4:
47.5kg (Fe is less than or equal to 0.1ppm) of purified aluminum potassium sulfate reacts with 26.6kg of potassium phosphate (Fe is less than or equal to 0.1ppm) to prepare an intermediate product, namely aluminum phosphate precipitate, and then the intermediate product reacts with 22.5kg of phosphoric acid with 85 percent of Fe being less than or equal to 1ppm to prepare aluminum dihydrogen phosphate solution. Thereafter, the same procedures as in example 1 were carried out, except that 25.2kg of the sample prepared in example 4 was assigned the reference numeral S4 and the yield thereof was 95%.
Example 5:
using ammonia water as a precipitator to prepare aluminum hydroxide precipitate from 45.3kg of purified aluminum ammonium sulfate (Fe is less than or equal to 0.1ppm), and reacting the aluminum ammonium sulfate with 33kg of phosphoric acid with the content of 85 percent and the Fe content of less than or equal to 1ppm after washing to prepare aluminum dihydrogen phosphate solution. The subsequent steps were the same as in example 1, with a muffle firing temperature of 610 ℃. 24.8kg of the sample prepared in example 5 has the designation S5. The one-time yield is about 94%, the particles are fine and uniform, the color is bright white, the Fe ion is less than 2ppm, and the Co, Ni and Cu are less than 1 ppm.
The products of the above examples 1 to 5 were tested, and the statistical analysis results are shown in the following table 1:
TABLE 1
As can be seen from the above examples and the results of the product component analysis, the method for preparing high-purity aluminum dihydrogen phosphate of the invention is simple, the operation is easy, the production cost is low, the quality of the obtained high-purity aluminum metaphosphate product is stable, the content is not less than 99.0%, the particles are fine and uniform, the product particles can pass through a 80-mesh sieve without being crushed by a crusher, the color is bright white, the content of non-ferrous metal ions is small, and the iron ions are iron ions<2ppm, and less than 1ppm of Co, Ni and Cu, and can be used for preparing optical glass and special glass materials. To further confirm that the product prepared by the preparation method is aluminum metaphosphate, the crystal structure of the aluminum metaphosphate powder obtained in example 5 was characterized by using an X-ray diffraction apparatus under the following conditions: the radiation source Cu target Ka ray, the tube voltage 40KV, the tube current 30mA, the scanning speed 6 deg/min, the scanning range 2 theta 5-90 deg. The results are shown in FIG. 1, which are substantially consistent with the standard card PDF 130430, and the molecular formula is Al (PO)3)3This shows that the product prepared by the preparation method has no sintering polymerization, is consistent with the phenomenon of test roasting, and is bulky and easy to crush.
Claims (1)
1. A preparation method of powdery high-purity aluminum metaphosphate suitable for optical glass is characterized by comprising the following steps:
(1) preparation of high purity aluminum compound precipitate: after purifying soluble aluminum salt, adding a precipitator to prepare high-purity aluminum compound precipitate;
(2) washing: boiling the aluminum compound precipitate prepared in the step (1), then carrying out heat preservation and sedimentation at 70-90 ℃, pouring supernatant, taking out slurry and carrying out centrifugal drying; putting the solid into an enamel pot, adding pure water, stirring to disperse, stirring to boil, keeping the temperature, settling, pouring the supernatant, centrifugally spin-drying the slurry, repeating for several times until the conductivity of the supernatant is less than or equal to 100 mus/cm, centrifugally spin-drying the slurry, and inspecting the content;
(3) and (3) dilution of phosphoric acid: selecting a phosphoric acid solution with the impurity Fe of less than or equal to 2ppm and the content of more than or equal to 85 percent to prepare a phosphoric acid solution with the concentration of 20-60 percent;
(4) preparation of aluminum dihydrogen phosphate solution: the phosphoric acid solution prepared in the step (3) is injected into a reaction kettle, heated to 70-80 ℃, and then completely reacted according to P contained in the final solution2O5/Al2O3Adding one or two of aluminum hydrogen phosphate, aluminum phosphate or aluminum hydroxide in a mass ratio of 4.0-4.4;
(5) removing impurities and assisting filtration by using activated carbon: when the concentration of the solution is concentrated to 30-33Be degrees, adding activated carbon into the aluminum dihydrogen phosphate solution prepared in the step (4) to adsorb impurities in the solution, thereby achieving the purpose of removing the impurities; the using amount of the activated carbon is 1-5 per mill of the volume of the solution, the time is 20-30 min, and the next step is carried out after the solution is subjected to filter pressing and cleaning;
(6) p in the filtered aluminum dihydrogen phosphate solution obtained in the step (5)2O5/Al2O3The mass ratio of the P-containing compound is finely adjusted when the P-containing compound is in the aluminum dihydrogen phosphate solution2O5/Al2O3If the mass ratio of the phosphoric acid to the aluminum phosphate is = 4.0-4.4, the next procedure can be carried out, otherwise, the phosphoric acid or the processed aluminum phosphate, aluminum hydrogen phosphate or aluminum hydroxide is supplemented according to the metering ratio, and the operation of the steps (5) and (6) is continued;
(7) evaporation concentration or spray drying: heating by using steam, evaporating and concentrating the solution obtained in the step (6) until a large amount of foams exist in the aluminum dihydrogen phosphate solution and a little white crystals are separated out, stopping heating, taking out and placing in a plastic barrel for cooling to obtain a very viscous solution; or directly spray-drying the solution obtained in the step (6) at the air inlet temperature of 200-240 ℃ to obtain aluminum dihydrogen phosphate powder;
(8) preparing aluminum metaphosphate by microwave heating: placing the aluminum dihydrogen phosphate viscous liquid or the aluminum dihydrogen phosphate powder obtained in the step (7) into a high-temperature-resistant and microwave-resistant ceramic vessel, placing the ceramic vessel into a microwave oven for microwave heating reaction, wherein the reaction time is determined by the amount of reaction materials, the moisture contained in the reaction materials and the microwave heating power, the reaction end point is that the materials generate a multi-gap, layered, foamed and fluffy white object, the materials are instantly and rapidly heated to more than 600 ℃ in the reaction process, and after the reaction is finished, cooling and taking out the materials;
(9) crushing aluminum metaphosphate: taking out the precursor of the aluminum metaphosphate prepared by the microwave oven reaction in the step (8), and crushing by using a ceramic rod to be uniform;
(10) and (3) roasting to prepare aluminum metaphosphate: putting the aluminum metaphosphate prepared in the step (9) into a muffle furnace, and roasting at 600-800 ℃;
(11) detection and packaging: sampling and detecting the aluminum metaphosphate obtained in the step (10), obtaining a qualified finished product, and packaging the finished product according to requirements to obtain a powdery high-purity aluminum metaphosphate finished product;
the soluble aluminum salt in the step (1) is aluminum chloride, aluminum sulfate, aluminum nitrate, aluminum ammonium sulfate or aluminum potassium sulfate;
the precipitator in the step (1) is selected from potassium phosphate, sodium phosphate, ammonium phosphate, potassium hydrogen phosphate, sodium hydrogen phosphate, ammonium hydrogen phosphate and ammonia water;
in the step (8), the power of the microwave oven is more than 1000W, and a high-fire function is adopted.
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