CN116082030A - Aluminum phosphate ceramic produced by using unpurified wet-process phosphoric acid, and method and application thereof - Google Patents

Aluminum phosphate ceramic produced by using unpurified wet-process phosphoric acid, and method and application thereof Download PDF

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CN116082030A
CN116082030A CN202211674525.4A CN202211674525A CN116082030A CN 116082030 A CN116082030 A CN 116082030A CN 202211674525 A CN202211674525 A CN 202211674525A CN 116082030 A CN116082030 A CN 116082030A
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aluminum phosphate
ceramic
weight
oxide
parts
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CN116082030B (en
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廖欢
李潇咏
黄科林
蓝丽红
余慧群
黄灏彬
蓝擎
侯欣怡
覃善丽
宁红
孙励耘
刘晗昱
朱志赓
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Guangxi Kecubic New Material Co ltd
Guangxi Kelin Chenglin Science & Technology Co ltd
Guangxi Institute Of New Functional Materials Co ltd
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Guangxi Kecubic New Material Co ltd
Guangxi Kelin Chenglin Science & Technology Co ltd
Guangxi Institute Of New Functional Materials Co ltd
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Abstract

The invention discloses a method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, which comprises the following steps: (1) preparing aluminum phosphate; (2) treating aluminum phosphate; (3) blank preparation; (4) glaze configuration; (5) preparing a ceramic blank; (6) glaze treatment is applied to the ceramic blank; (7) high temperature calcination of the sample. In the invention, impurity ions such as fluorine, sulfate radical, iron, arsenic and the like are treated in the process, and the impurities are not required to be converted and separated, so that the working procedure is simplified, and the energy consumption is saved; and aluminum phosphate is manufactured into aluminum phosphate ceramic so as to improve extreme environment resistance of the aluminum phosphate ceramic and obtain a high-performance aluminum phosphate ceramic product. The process of the invention can effectively improve the design flexibility of the material, so that the ceramic has higher dimensional stability and can greatly reduce the cost.

Description

Aluminum phosphate ceramic produced by using unpurified wet-process phosphoric acid, and method and application thereof
[ field of technology ]
The invention belongs to the field of advanced ceramic preparation, and relates to aluminum phosphate ceramic produced by using unpurified wet-process phosphoric acid, and a method and application thereof.
[ background Art ]
After the wet-process phosphoric acid is purified and decontaminated by a proper method, the purity and impurity content of the product can be compared with those of the hot-process phosphoric acid, but the purification process is complex, the energy consumption is high, and the production cost is close to that of the hot-process phosphoric acid. Advanced ceramics, also called high performance ceramics, fine ceramics, high technology ceramics, etc., are ceramics which are prepared by adopting high-purity, superfine artificial synthesis or carefully selected inorganic compounds as raw materials and have excellent mechanical, acoustic, optical, thermal, electric, biological and other characteristics. The advanced ceramic is different from the traditional ceramic in the aspects of raw materials and processes, and the specific fine structure ensures that the advanced ceramic has a series of advantages of high strength, high hardness, wear resistance, corrosion resistance, high temperature resistance, insulation, superconductivity, biocompatibility and the like, is widely applied to the fields of national defense, chemical industry, metallurgy, electronics, machinery, aviation, aerospace, biomedicine and the like, and is one of industries which mainly support development in China in recent years. Aluminum phosphate is one of the raw materials of advanced ceramic materials and is also a high-end downstream product of the phosphorus chemical industry, and the higher the purification degree of the aluminum phosphate is, the higher the thermal stability, the excellent mechanical property and weather resistance and the thermochemical stability of the ceramic can be realized by applying the aluminum phosphate to the ceramic. At present, aluminum phosphate used for ceramic binders in China is usually manufactured by adopting hot phosphoric acid or wet purification phosphoric acid; the raw wet-process phosphoric acid does not meet the requirements of advanced ceramic use.
For example, in the Chinese patent application publication No. CN108455995A, a silicon carbide fiber reinforced aluminum phosphate ceramic matrix composite material and a preparation method thereof are disclosed, wherein a silicon carbide fiber cloth which is subjected to photoresist removal treatment and drying is put into a polyamic acid solution for dipping, and is solidified to obtain a silicon carbide fiber cloth containing an antioxidant coating; uniformly coating aluminum phosphate slurry on the outer surfaces of a plurality of pieces of silicon carbide fiber cloth containing an antioxidant coating, laminating the silicon carbide fiber cloth coated with the aluminum phosphate slurry, and then carrying out vacuum impregnation and mould pressing to obtain the silicon carbide fiber reinforced aluminum phosphate ceramic matrix composite material, so that the strength and toughness of the composite material are improved, and the high mechanical property can be maintained under a high-temperature anaerobic environment.
The Chinese patent application document "a method for preparing high closed porosity quartz-aluminum phosphate ceramic (publication No. CN 108484222A)", which is characterized in that aluminum dihydrogen phosphate and aluminum nitrate mixed solution are dripped on the surface of porous quartz and can be inhaled into the porous quartz, after drying, aluminum dihydrogen phosphate and aluminum nitrate form a thin layer on the surface of the porous ceramic, a continuous and complete liquid film can be formed outside the surface of the porous ceramic in the sintering process, and open pores are sealed, so that the closed porosity of the porous ceramic can be remarkably improved.
There are no reports in the prior art about the technological process for manufacturing aluminum phosphate ceramics by using wet phosphoric acid and the good effect; the application of aluminum phosphate to ceramic and other materials can improve the high temperature resistance, chemical corrosion resistance, strong impact resistance and other properties of the corresponding materials, and meanwhile, practical results show that the application of the unpurified wet aluminum phosphate to ceramic systems can lead to poor performance such as compressive strength, flexural strength and the like, iron ions and the like in the aluminum phosphate play a role in catalysis, so that the viscosity of the system is increased sharply after the phosphoric acid is heated, crystals are difficult to separate out, the purity of the aluminum phosphate is further influenced, and the content of free impurity ions is higher, especially iron, arsenic, fluoride ions, sulfate ions and the like, so that the coarser and more uneven particles of the aluminum phosphate are caused, the performance is greatly reduced and the bad rate of the ceramic is increased when the aluminum phosphate is applied to advanced ceramics.
[ invention ]
In order to overcome the defects and shortcomings of the prior art, the invention provides aluminum phosphate ceramic produced by using unpurified wet-process phosphoric acid, and a method and application thereof, so as to obtain a high-performance aluminum phosphate ceramic product.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, comprising the following steps:
(1) Preparing aluminum phosphate by using unpurified wet phosphoric acid and aluminum hydroxide;
(2) Treating aluminum phosphate by using a chemical reaction method, a physical adsorption method or a crystallization method;
(3) Preparing a blank: preparing a blank ceramic slurry from 60-80 parts by weight of composite oxide, 20-40 parts by weight of aluminum phosphate and 1-5 parts by weight of dispersing agent a;
(4) Glaze configuration: preparing glaze ceramic slurry by 30-50 parts by weight of oxide, 50-70 parts by weight of aluminum phosphate and 0.5-5 parts by weight of dispersant b;
(5) Placing the blank ceramic slurry into a compression molding die, and adopting compression molding to prepare a ceramic blank;
(6) Drying the ceramic blank obtained in the step (5) for 1-6 hours at 60-90 ℃ and then uniformly applying glaze on the blank to obtain a sample;
(7) And (3) placing the sample obtained in the step (6) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 300-1800 ℃, and obtaining the aluminum phosphate ceramic.
Further, the chemical reaction method in the step (2) is to add a chemical agent which reacts with impurity ions to generate solid precipitate into the aluminum phosphate solution, and solidify the iron, arsenic and fluorine ion precipitate in the aluminum phosphate; the chemical agent comprises one or more than two of barium sulfide, sodium hydrosulfide, aluminum sulfate and calcium hydroxide.
Further, the adsorption method in the step (2) is to adsorb and fix iron, sulfate radical and fluorine in the aluminum phosphate solution by using an adsorbent according to the saturation difference of iron ions at different temperatures; the adsorbent comprises one or more than two of sodium alginate, activated carbon fiber, activated alumina, porous silica and ion exchange resin.
Further, the crystallization method in the step (2) is to prepare saturated solution of the adsorbed aluminum phosphate, keep stand for 12-48 hours, filter, obtain aluminum phosphate crystal after solid-liquid separation, dry and crush at 95 ℃.
Further, the composite oxide in the step (3) includes BaTiO 3 、SrTiO 3 、CaTiO 3 、MgTiO 3 、BaZrO 3 、SrZrO 3 、BaSnO 3 、CaSnO 3 、MgAl 2 O 3 、3Al 2 O 3 ·2SiO 2 One or two or more of them.
Further, the dispersing agent a in the step (3) and the dispersing agent b in the step (4) comprise one or more than two of sodium tripolyphosphate, sodium pyrophosphate, polyether, polypropylene olefin, polyacrylate, polyamine, polyalcohol, water glass, sodium hexametaphosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate, methylpentanol, sodium hydroxymethyl cellulose, polyacrylamide, ethyl distearate and sodium stearate.
Further, the oxide in the step (4) includes one or more of sodium oxide, potassium oxide, aluminum oxide, silicon oxide, beryllium oxide, titanium oxide, magnesium oxide, calcium oxide, zinc oxide, barium oxide, zirconium oxide, and strontium oxide.
Preferably, the crystallization method in the step (2) is allowed to stand for 12 to 48 hours. In a preferred embodiment, the rest time is 24 hours.
Preferably, in the step (5), the pressure of compression molding is 4 to 8MPa. In a preferred embodiment, compression molding is used at a pressure of 6MPa.
Preferably, in the step (6), the drying temperature of the ceramic green body is 70-80 ℃. In a preferred embodiment, the ceramic green body is dried at 80 ℃.
Preferably, in the step (6), the ceramic green body is dried for 3 to 5 hours. In a preferred embodiment, the ceramic green body is dried for 4 hours.
Preferably, in the step (7), the sample obtained in the step (6) is calcined in a high temperature furnace at a high temperature of 800 to 1200 ℃. In a preferred embodiment, the sample obtained in step (6) is cured at a high temperature in a high temperature oven at a curing temperature of 900 ℃.
The invention has the following beneficial effects:
(1) The raw materials for producing the aluminum phosphate ceramic are matched with each other, and the flexural strength, the breakdown strength, the chemical corrosion resistance, the high temperature resistance and the like of the product are synergistically improved.
(2) In the invention, impurity ions such as fluorine, sulfate radical, iron, arsenic and the like are treated in the process, and the impurities are not required to be converted and separated, so that the working procedure is simplified, and the energy consumption is saved; and aluminum phosphate is manufactured into aluminum phosphate ceramics so as to improve extreme environmental resistance of the aluminum phosphate ceramics: the high-performance aluminum phosphate ceramic product is obtained by the properties of flexural strength, breakdown strength, chemical corrosion resistance, high temperature resistance, low linear expansion coefficient and the like.
(3) Compared with the prior art, the aluminum phosphate ceramic product has higher flexural strength and breakdown strength, can resist high temperature of more than 1000 ℃, has smaller loss of hydrochloric acid and sodium hydroxide, has better extreme resistance and lower linear expansion coefficient, and can be widely applied to the fields of national defense, chemical industry, metallurgy, electronics, machinery, aviation, aerospace, biomedicine and the like.
(4) The invention improves the design flexibility of the material, ensures that the ceramic has higher dimensional stability and can effectively reduce the cost.
[ detailed description ] of the invention
For a better understanding of the present invention, reference is made to the following examples, which are included within the scope of the present invention, but are not intended to limit the scope of the present invention.
Example 1
A method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, comprising the following steps: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. circulating barium sulfide and sodium hydrosulfide in the aluminum phosphate solution to form precipitate of iron ions and arsenic ions in the aluminum phosphate; 3. adjusting the aluminum phosphate solution obtained in the step 2 to 56.7 ℃ and 64 ℃, separating out iron ions in the aluminum phosphate solution according to the saturation difference of the iron ions at the two temperatures, and adsorbing with an activated alumina and sodium alginate adsorbent; 4. preparing the adsorbed aluminum phosphate into a saturated solution, standing for 24 hours, filtering, performing solid-liquid separation to obtain an aluminum phosphate crystal, and drying and crushing at 95 ℃ to prepare aluminum phosphate; 5. 30 parts by weight of BaTiO 3 20 parts by weight of MgAl 2 O 3 10 parts by weight of 3Al 2 O 3 ·2SiO 2 Preparing green ceramic slurry by 40 parts by weight of aluminum phosphate, 1 part by weight of high-purity sodium phosphate and 1 part by weight of aluminum hexametaphosphate; 6. 5 parts by weight of sodium oxide, 10 parts by weight of barium oxide, 10 parts by weight of silicon oxide, 5 parts by weight ofPreparing ceramic glaze slurry by calcium oxide, 1 part by weight of triethylhexyl phosphoric acid, 1 part by weight of sodium dodecyl sulfate and 70 parts by weight of high-purity aluminum phosphate; 7. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 8. drying the ceramic blank obtained in the step 7 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 9. and (3) placing the sample obtained in the step (8) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 900 ℃, and obtaining the aluminum phosphate ceramic.
Example 2
A method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, comprising the following steps: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. circulating barium sulfide and sodium hydrosulfide in the aluminum phosphate solution, and removing iron ions and arsenic ions in the aluminum phosphate by precipitation; 3. adjusting the aluminum phosphate solution obtained in the step 2 to 56.7 ℃ and 64 ℃, separating out iron ions in the aluminum phosphate solution according to the saturation difference of the iron ions at the two temperatures, and removing the iron ions by using sodium alginate and activated carbon adsorbent; 4. preparing the adsorbed aluminum phosphate into a saturated solution, standing for 24 hours, filtering, performing solid-liquid separation to obtain an aluminum phosphate crystal, and drying and crushing at 95 ℃ to prepare aluminum phosphate; 5. 30 parts by weight of SrTiO 3 25 parts by weight of MgTiO 3 15 parts by weight of BaSnO 3 Preparing green ceramic slurry by 30 parts by weight of high-purity aluminum phosphate, 1% by weight of sodium hydroxymethyl cellulose and 1 part by weight of polyether; 6. preparing ceramic glaze slurry from 5 parts by weight of zirconium oxide, 10 parts by weight of aluminum oxide, 10 parts by weight of beryllium oxide, 5 parts by weight of titanium oxide, 1 part by weight of polyacrylamide, 1 part by weight of ethyl distearate and 70 parts by weight of high-purity aluminum phosphate; 7. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 8. drying the ceramic blank obtained in the step 7 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 9. and (3) placing the sample obtained in the step (8) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 1100 ℃, and obtaining the aluminum phosphate ceramic.
Example 3
A method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, comprising the following steps: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. circulating barium sulfide and sodium hydrosulfide in the aluminum phosphate solution, and removing iron ions and arsenic ions in the aluminum phosphate by precipitation; 3. adjusting the aluminum phosphate solution obtained in the step 2 to 56.7 ℃ and 64 ℃, separating out iron ions in the aluminum phosphate solution according to the saturation difference of the iron ions at the two temperatures, and removing the iron ions by using activated carbon and activated carbon fiber adsorbent; 4. preparing the adsorbed aluminum phosphate into a saturated solution, standing for 24 hours, filtering, performing solid-liquid separation to obtain an aluminum phosphate crystal, and drying and crushing at 95 ℃ to prepare aluminum phosphate; 5. 30 parts by weight of BaTiO 3 25 parts by weight of SrTiO 3 10 parts by weight of BaZrO 3 10 parts by weight of CaSnO 3 Preparing green ceramic slurry by 20 parts by weight of aluminum phosphate, 1 part by weight of polypropylene and 1 part by weight of polyether; 6. preparing ceramic glaze slurry by 10 parts by weight of magnesium oxide, 15 parts by weight of aluminum oxide, 10 parts by weight of silicon oxide, 5 parts by weight of titanium oxide, 1 part by weight of polyacrylate, 1 part by weight of polyol and 60 parts by weight of aluminum phosphate; 7. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 8. drying the ceramic blank obtained in the step 7 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 9. and (3) placing the sample obtained in the step (8) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 1500 ℃, and obtaining the aluminum phosphate ceramic.
Example 4
A method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, comprising the following steps: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. circulating barium sulfide and sodium hydrosulfide in the aluminum phosphate solution, and removing iron ions and arsenic ions in the aluminum phosphate by precipitation; 3. adjusting the aluminum phosphate solution obtained in the step 2 to 56.7 ℃ and 64 ℃, separating out iron ions in the aluminum phosphate solution according to the saturation difference of the iron ions at the two temperatures, and removing the iron ions by using porous silica and an activated carbon adsorbent; 4. adsorbing the adsorbed aluminum phosphatePreparing saturated solution, standing for 24 hours, filtering, separating solid from liquid to obtain aluminum phosphate crystals, drying at 95 ℃, and pulverizing to obtain aluminum phosphate; 5. 20 parts by weight of MgTiO 3 20 parts by weight of BaZrO 3 15 parts by weight of BaSnO 3 15 parts by weight of SrZrO 3 Preparing green ceramic slurry by 30 parts by weight of high-purity aluminum phosphate, 1 part by weight of polyacrylate and 2 parts by weight of sodium pyrophosphate; 6. preparing ceramic glaze slurry from 15 parts by weight of magnesium oxide, 15 parts by weight of titanium oxide, 10 parts by weight of silicon oxide, 5 parts by weight of zinc oxide, 5 parts by weight of sodium oxide, 2 parts by weight of methylpentanol, 2 parts by weight of polyamine and 50 parts by weight of high-purity aluminum phosphate; 7. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 8. drying the ceramic blank obtained in the step 7 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 9. and (3) placing the sample obtained in the step (8) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 1250 ℃, and obtaining the high-purity aluminum phosphate ceramic.
Example 5
A method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, comprising the following steps: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. circulating barium sulfide and sodium hydrosulfide in the aluminum phosphate solution, and removing iron ions and arsenic ions in the aluminum phosphate by precipitation; 3. adjusting the aluminum phosphate solution obtained in the step 2 to 56.7 ℃ and 64 ℃, separating out iron ions in the aluminum phosphate solution according to the saturation difference of the iron ions at the two temperatures, and removing the iron ions by using sodium alginate and activated carbon fiber adsorbent; 4. preparing the adsorbed aluminum phosphate into a saturated solution, standing for 24 hours, filtering, performing solid-liquid separation to obtain an aluminum phosphate crystal, and drying and crushing at 95 ℃ to prepare aluminum phosphate; 5. 25 parts by weight of CaTiO 3 25 parts by weight of SrZrO 3 20 parts by weight of MgAl 2 O 3 10 parts by weight of 3Al 2 O 3 ·2SiO 2 Preparing green ceramic slurry by 20 parts by weight of aluminum phosphate, 2 parts by weight of polyacrylate and 2 parts by weight of calcium stearate; 6. 15 parts by weight of sodium oxide15 parts by weight of titanium oxide, 10 parts by weight of silicon oxide, 10 parts by weight of aluminum oxide, 5 parts by weight of polyether and 60 parts by weight of aluminum tripolyphosphate to prepare ceramic glaze slurry; 7. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 8. drying the ceramic blank obtained in the step 7 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 9. and (3) placing the sample obtained in the step (8) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 1600 ℃, and obtaining the aluminum phosphate ceramic.
Example 6
A method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, comprising the following steps: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. circulating barium sulfide and sodium hydrosulfide in the aluminum phosphate solution, and removing iron ions and arsenic ions in the aluminum phosphate by precipitation; 3. adjusting the aluminum phosphate solution obtained in the step 2 to 56.7 ℃ and 64 ℃, separating out iron ions in the aluminum phosphate solution according to the saturation difference of the iron ions at the two temperatures, and removing the iron ions by using sodium alginate, activated carbon and activated carbon cellulose adsorbent; 4. preparing the adsorbed aluminum phosphate into a saturated solution, standing for 24 hours, filtering, performing solid-liquid separation to obtain an aluminum phosphate crystal, and drying and crushing at 95 ℃ to prepare aluminum phosphate; 5. 25 parts by weight of SrTiO 3 MgTiO 20 parts by weight 3 15 parts by weight of CaSnO 3 Preparing green ceramic slurry by 30 parts by weight of high-purity aluminum phosphate and 3 parts by weight of polypropylene; 6. preparing ceramic glaze slurry by 15 parts by weight of sodium oxide, 10 parts by weight of potassium oxide, 15 parts by weight of silicon oxide, 4 parts by weight of polyol and 70 parts by weight of high-purity aluminum phosphate; 7. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 8. drying the ceramic blank obtained in the step 7 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 9. and (3) placing the sample obtained in the step (8) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 550 ℃, and obtaining the aluminum phosphate ceramic.
Comparative example 1
Raw aluminum phosphate ceramicA method of production comprising the steps of: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. 30 parts by weight of BaTiO 3 25 parts by weight of SrTiO 3 10 parts by weight of BaZrO 3 10 parts by weight of CaSnO 3 Preparing green ceramic slurry by 20 parts by weight of aluminum phosphate, 1 part by weight of polypropylene and 1 part by weight of polyether; 3. preparing ceramic glaze slurry by 10 parts by weight of magnesium oxide, 15 parts by weight of aluminum oxide, 10 parts by weight of silicon oxide, 5 parts by weight of titanium oxide, 1 part by weight of polyacrylate, 1 part by weight of polyol and 60 parts by weight of aluminum phosphate; 4. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 5. drying the ceramic blank obtained in the step 4 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 6. and (3) placing the sample obtained in the step (5) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 900 ℃, and obtaining the aluminum phosphate ceramic.
Comparative example 2
A method for producing aluminum phosphate ceramics, comprising the following steps: 1. preparing aluminum phosphate by using unpurified wet-process phosphoric acid; 2. 25 parts by weight of CaTiO 3 25 parts by weight of SrZrO 3 20 parts by weight of MgAl 2 O 3 10 parts by weight of 3Al 2 O 3 ·2SiO 2 Preparing green ceramic slurry by 20 parts by weight of aluminum phosphate, 2 parts by weight of polyacrylate and 2 parts by weight of calcium stearate; 3. preparing ceramic glaze slurry from 15 parts by weight of sodium oxide, 15 parts by weight of titanium oxide, 10 parts by weight of silicon oxide, 10 parts by weight of aluminum oxide, 5 parts by weight of polyether and 60 parts by weight of aluminum tripolyphosphate; 4. placing the blank ceramic slurry into a compression molding die, and adopting compression molding, wherein the compression molding pressure is 6MPa, so as to prepare a ceramic blank; 5. drying the ceramic blank obtained in the step 4 for 4 hours at 80 ℃, and uniformly applying glaze on the blank to obtain a sample; 6. and (3) placing the sample obtained in the step (5) in a high-temperature furnace for high-temperature curing, wherein the curing temperature is 900 ℃, and obtaining the aluminum phosphate ceramic.
Test example 3, example 5, comparative example 1, comparative example 2 flexural strength, breakdown strength, soak (1+9) hydrochloric acid loss, soak 10% hydrogenSodium oxide loss, high temperature resistance, linear expansion coefficient and other performances; the test standard of the flexural strength and the breakdown strength is national standard GB/T5593-2015 ceramic materials for electronic components; the test standard of the linear expansion coefficient is national standard GB/T5594.3-2015, part 3 of the test method for the ceramic material performance of the electronic component structure, average linear expansion coefficient test method; high temperature resistance test standard GB/T5593-2015 ceramic Material for electronic components; soaking (1+9) hydrochloric acid loss and 10% sodium hydroxide loss test standard GB/T5594.6-2015, chemical stability test method, part 6 of ceramic Material Performance test method for electronic component Structure. Material performance rating criteria: the flexural strength is more than or equal to 80Mpa, the breakdown strength is more than or equal to 18kV/mm, and the loss of hydrochloric acid soaked in (1+9) is less than or equal to 0.7mg/cm 2 The loss of 10% sodium hydroxide after soaking is less than or equal to 0.2mg/cm 2 The high temperature resistance is more than or equal to 800 ℃, and the linear expansion coefficient (20-800 ℃) is less than or equal to 8 multiplied by 10 -6 /℃。
Figure BDA0004017624900000121
Figure BDA0004017624900000131
From the above table: compared with comparative examples 1 and 2, the examples 3 and 5 have higher flexural strength and breakdown strength, can resist high temperature up to more than 1000 ℃, have smaller loss of hydrochloric acid and sodium hydroxide, and have better extreme resistance; the lower linear expansion coefficient improves the design flexibility of the material, leads the ceramic to have higher dimensional stability and can reduce the cost. Therefore, the raw materials for producing the aluminum phosphate ceramic are matched with each other, so that the aluminum phosphate prepared by the scheme can ensure that the ceramic has more excellent performance, the rupture strength, the breakdown strength, the chemical corrosion resistance, the high temperature resistance and the like of the product are synergistically improved, and the technology of the invention has remarkable progress.
It should not be considered that the implementation of the invention is limited to these descriptions, but that it is possible for a person skilled in the art to which the invention pertains to make several simple deductions or substitutions without departing from the idea of the invention, all of which should be considered as belonging to the scope of protection of the invention as defined in the appended claims.

Claims (10)

1. A method for producing aluminum phosphate ceramics by using unpurified wet-process phosphoric acid, which is characterized by comprising the following steps:
(1) Preparing aluminum phosphate by using unpurified wet phosphoric acid and aluminum hydroxide;
(2) Treating aluminum phosphate by using a chemical reaction method, a physical adsorption method or a crystallization method;
(3) Preparing a blank: preparing a blank ceramic slurry from 60-80 parts by weight of composite oxide, 20-40 parts by weight of aluminum phosphate and 1-5 parts by weight of dispersing agent a;
(4) Glaze configuration: preparing glaze ceramic slurry by 30-50 parts by weight of oxide, 50-70 parts by weight of aluminum phosphate and 0.5-5 parts by weight of dispersant b;
(5) Placing the blank ceramic slurry into a compression molding die, and adopting compression molding to prepare a ceramic blank;
(6) Drying the ceramic blank obtained in the step (5) for 1-6 hours at 60-90 ℃ and then uniformly applying glaze on the blank to obtain a sample;
(7) And (3) placing the sample obtained in the step (6) in a high-temperature furnace for high-temperature calcination, wherein the calcination temperature is 300-1800 ℃, and obtaining the aluminum phosphate ceramic.
2. The method for producing aluminum phosphate ceramic by using raw wet process phosphoric acid according to claim 1, wherein the chemical reaction method in the step (2) is to add chemical agent which reacts with impurity ions to generate solid precipitate into aluminum phosphate solution, and solidify iron, arsenic and fluorine ions in aluminum phosphate precipitate; the chemical agent comprises one or more than two of barium sulfide, sodium hydrosulfide, aluminum sulfate and calcium hydroxide.
3. The method for producing aluminum phosphate ceramic by using raw wet process phosphoric acid according to claim 1, wherein the adsorption method in the step (2) is to adsorb and fix iron, sulfate radical and fluorine in the aluminum phosphate solution by using adsorbents according to the saturation difference of iron ions at different temperatures; the adsorbent comprises one or more than two of sodium alginate, activated carbon fiber, activated alumina, porous silica and ion exchange resin.
4. The method for producing aluminum phosphate ceramic by using raw wet process phosphoric acid according to claim 1, wherein the crystallization method in the step (2) is to prepare saturated solution of adsorbed aluminum phosphate, keep the solution stand for 12-48 hours, filter the solution, obtain aluminum phosphate crystal after solid-liquid separation, and dry and crush the aluminum phosphate crystal.
5. The method for producing aluminum phosphate ceramic using raw wet process phosphoric acid according to claim 1, wherein the composite oxide in the step (3) comprises BaTiO 3 、SrTiO 3 、CaTiO 3 、MgTiO 3 、BaZrO 3 、SrZrO 3 、BaSnO 3 、CaSnO 3 、MgAl 2 O 3 、3Al 2 O 3 ·2SiO 2 One or two or more of them.
6. The method for producing aluminum phosphate ceramic using raw wet process phosphoric acid according to claim 1, wherein the dispersant a in the step (3) and the dispersant b in the step (4) comprise one or more of sodium tripolyphosphate, sodium pyrophosphate, polyether, polypropylene olefin, polyacrylate, polyamine, polyol, water glass, sodium hexametaphosphate, triethylhexyl phosphoric acid, sodium dodecyl sulfate, methylpentanol, sodium hydroxymethyl cellulose, polyacrylamide, ethyl distearate, and sodium stearate.
7. The method for producing aluminum phosphate ceramic using raw wet process phosphoric acid according to claim 1, wherein the oxide in the step (4) comprises one or more of sodium oxide, potassium oxide, aluminum oxide, silicon oxide, beryllium oxide, titanium oxide, magnesium oxide, calcium oxide, zinc oxide, barium oxide, zirconium oxide, and strontium oxide.
8. The method for producing aluminum phosphate ceramic using raw wet process phosphoric acid according to claim 1, wherein in the step (5), a pressure of 4 to 8MPa is used for compression molding.
9. An aluminum phosphate ceramic produced according to the method of any one of claims 1-8.
10. Use of an aluminium phosphate ceramic according to claim 9, wherein the field of application of aluminium phosphate ceramic comprises national defense, chemical, metallurgical, electronic, mechanical, aeronautical, astronautical, biomedical.
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