CN115340076B - Preparation method of yttrium phosphate - Google Patents
Preparation method of yttrium phosphate Download PDFInfo
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- CN115340076B CN115340076B CN202210871671.XA CN202210871671A CN115340076B CN 115340076 B CN115340076 B CN 115340076B CN 202210871671 A CN202210871671 A CN 202210871671A CN 115340076 B CN115340076 B CN 115340076B
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- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 title claims abstract description 103
- UXBZSSBXGPYSIL-UHFFFAOYSA-K yttrium(iii) phosphate Chemical compound [Y+3].[O-]P([O-])([O-])=O UXBZSSBXGPYSIL-UHFFFAOYSA-K 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 88
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052742 iron Inorganic materials 0.000 claims abstract description 44
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 39
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 30
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 28
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 13
- 239000013078 crystal Substances 0.000 claims abstract description 13
- AUYOHNUMSAGWQZ-UHFFFAOYSA-L dihydroxy(oxo)tin Chemical compound O[Sn](O)=O AUYOHNUMSAGWQZ-UHFFFAOYSA-L 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 62
- 239000000243 solution Substances 0.000 claims description 42
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 31
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 31
- 229910052793 cadmium Inorganic materials 0.000 claims description 31
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 31
- 229910052804 chromium Inorganic materials 0.000 claims description 31
- 239000011651 chromium Substances 0.000 claims description 31
- 229910017052 cobalt Inorganic materials 0.000 claims description 31
- 239000010941 cobalt Substances 0.000 claims description 31
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 31
- 229910052802 copper Inorganic materials 0.000 claims description 31
- 239000010949 copper Substances 0.000 claims description 31
- 229910052759 nickel Inorganic materials 0.000 claims description 31
- 229910052720 vanadium Inorganic materials 0.000 claims description 31
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 31
- 239000012498 ultrapure water Substances 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 20
- 239000012065 filter cake Substances 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 239000005304 optical glass Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 4
- 238000007865 diluting Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 239000012535 impurity Substances 0.000 abstract description 22
- 239000006227 byproduct Substances 0.000 abstract description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 2
- 238000001556 precipitation Methods 0.000 abstract description 2
- 238000004062 sedimentation Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 22
- 239000002994 raw material Substances 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 5
- 238000003556 assay Methods 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 239000010413 mother solution Substances 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 229910009523 YCl3 Inorganic materials 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- KGIXBJYLGFKRAA-UHFFFAOYSA-K dihydrogen phosphate yttrium(3+) Chemical compound [Y+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O KGIXBJYLGFKRAA-UHFFFAOYSA-K 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 150000003746 yttrium Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/04—Opacifiers, e.g. fluorides or phosphates; Pigments
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C3/00—Fertilisers containing other salts of ammonia or ammonia itself, e.g. gas liquor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
In order to solve the technical problem that the existing preparation method is difficult to produce high-purity yttrium phosphate in a mass mode, the invention provides the preparation method of yttrium phosphate, which comprises the steps of firstly dissolving yttrium oxide by hydrochloric acid to obtain yttrium chloride solution, removing heavy metal impurities in the solution by means of metastannic acid adsorption, removing iron impurities by hydrochloric acid with the mass fraction of 1.5-2.5%, and obtaining pure yttrium chloride solution after sedimentation and filtration. Further, adding diluted phosphoric acid solution into the yttrium chloride solution after impurity removal, wherein the byproduct is hydrochloric acid due to the reaction of phosphoric acid and yttrium chloride, and yttrium phosphate is basically dissolved in the hydrochloric acid, so that the precipitation is less, the yttrium phosphate can be directly used as seed crystal, a small amount of ammonia water is added to neutralize a small amount of hydrochloric acid to prepare yttrium phosphate seed crystal, then ammonia water is continuously added, and particles are formed after full reaction, so that yttrium phosphate synthetic solution is obtained; and dehydrating the obtained yttrium phosphate synthetic solution, and adopting a special gradient drying process to obtain yttrium phosphate with purity of more than 99.9%.
Description
Technical Field
The invention relates to a preparation method of yttrium phosphate.
Background
The yttrium phosphate is mainly applied to special ceramics, fluorescent materials and special optical glass, the optical glass added with the yttrium phosphate shows special light property and refractive index, but the required indexes are quite strict, wherein iron, cobalt, nickel, copper, cadmium, chromium and vanadium are required to be less than 0.5ppm, so that manufacturers for producing high-purity yttrium phosphate are rarely available on the market at present, most of the optical glass is laboratory products, and the optical glass is difficult to produce in a large quantity. However, with the rapid development of the optical glass industry, the demand for high-purity yttrium phosphate is increasing, so a preparation method of high-purity yttrium phosphate is needed to meet the increasing demand.
Disclosure of Invention
In order to solve the technical problem that the existing preparation method is difficult to produce high-purity yttrium phosphate in a large quantity, the invention provides the preparation method of yttrium phosphate, and yttrium phosphate with purity reaching more than 99.9% can be produced.
The technical scheme of the invention is as follows:
The preparation method of the yttrium phosphate is characterized by comprising the following steps of:
Step 1, yttrium salt purification
Diluting analytically pure hydrochloric acid to 15-22% by mass fraction with high-purity water, adding yttrium oxide into the solution, heating to 70-75 ℃ and stirring for reaction for 30-60 minutes, dissolving to be transparent, adding high-purity water to dilute to 1.1-1.12, adding metastannic acid and hydrochloric acid with the mass fraction of 1.5-2.5% into the reaction solution, adding 1/500-1/1000 of the mass fraction of the metastannic acid, fully stirring, settling, filtering supernatant, and controlling the contents of iron, cobalt, nickel, copper, cadmium, chromium and vanadium in the supernatant to be less than 0.1ppm to obtain a pure yttrium chloride solution; the reaction equation: y 2O3+6HCl＝YCl3+3H2 O; in the step, excessive metal impurities are adsorbed and settled through metastannic acid, and the removal effect of iron is enhanced through hydrochloric acid with the mass fraction of 1.5-2.5%;
step 2, synthesizing yttrium phosphate
Step 2.1, food grade phosphoric acid is centrally controlled until the contents of iron, cobalt, nickel, copper, cadmium, chromium and vanadium are all less than 0.1ppm, water is added for dilution until the mass fraction is 15-20%, the mixture is added into yttrium chloride solution, and the mixture is stirred and heated to 70-80 ℃; the reaction equation: YCl 3+H3PO4＝YPO4 +3HCl;
2.2, the reagent grade ammonia water is centrally controlled until the iron, cobalt, nickel, copper, cadmium, chromium and vanadium contents are less than 0.1ppm, the reagent grade ammonia water is diluted by adding high-purity water until the mass fraction is 8-9.5%, a small part of diluted ammonia water is firstly added into the synthetic liquid in the step 2.1, the temperature is kept at 85-90 ℃ for stirring reaction for 30-60 minutes to prepare seed crystals, the diluted ammonia water is continuously added into the synthetic liquid, the PH value is adjusted to 2.5-3.5, and the temperature is kept at 85-90 ℃ for stirring reaction for 2-3 hours to enable particles to be fully formed, so that yttrium phosphate synthetic liquid is obtained; as the yttrium chloride and phosphoric acid in the last step react to generate hydrochloric acid, most of yttrium phosphate can be dissolved into the hydrochloric acid, ammonia water is added to neutralize the hydrochloric acid, so that the hydrochloric acid is converted into ammonium chloride, and yttrium phosphate is separated out from the hydrochloric acid; the pH is adjusted to 2.5-3.5 to prevent hydrolysis of yttrium phosphate and to minimize/prevent formation of yttrium phosphate monobasic and/or monobasic;
Step 3, dehydrating and drying yttrium phosphate
Step 3.1, filter-pressing yttrium phosphate synthetic liquid, and then washing until the PH is 5-6 (at the moment, the mass fraction of chloride ions in the mother liquid is less than 0.02%), so as to obtain yttrium phosphate filter cake;
step 3.2, carrying out gradient drying on the yttrium phosphate filter cake:
a first gradient: drying at 200-300 deg.c for 2-3 hr;
A second gradient: and (3) drying at 500-600 ℃ for 2-3 hours to obtain yttrium phosphate. The purity of the product is higher than 99.9%, the iron content is less than 1ppm, the cobalt content, the nickel content, the copper content, the cadmium content, the chromium content and the vanadium content are all less than 0.5ppm, and the phosphorus pentoxide content is 38.5+/-1%.
Further, the impurity removing effect is best when the high purity water is added to dilute the mixture to a specific gravity of 1.1 in the step 1.
Further, in order to form better seed crystal, ammonia water with a theoretical mass of 1/10-1/15 is added into the synthetic liquid in the step 2.1 in the step 2.2.
Further, in order to prevent the formation of yttrium dihydrogen phosphate and yttrium dihydrogen phosphate, the PH is adjusted to 2.7 in step 2.2.
Further, the step 3.1 specifically comprises: pumping the yttrium phosphate synthetic solution into a plate-and-frame filter press, and adopting filter cloth with more than 1500 meshes to filter-press, washing with water until the PH is 5-6, thus obtaining yttrium phosphate filter cakes.
The high-purity yttrium phosphate is characterized in that: the preparation method is adopted.
An optical glass is characterized in that: the high-purity yttrium phosphate is added in the glass melting process.
The beneficial effects of the invention are as follows:
1. the invention adopts the easily-obtained yttrium oxide as the main raw material, and considers that if the yttrium oxide and phosphoric acid are directly synthesized, the purity of the obtained yttrium phosphate is insufficient, and the impurity metal index is higher. The method adopts a multistage conversion mode, firstly adopts hydrochloric acid to dissolve yttrium oxide to obtain yttrium chloride solution, adopts metastannic acid as an adsorbent to adsorb and remove heavy metal impurities in the solution because the yttrium chloride solution is acidic, and simultaneously adopts hydrochloric acid with the mass fraction of 1.5-2.5% to remove iron impurities, and can obtain pure yttrium chloride solution after sedimentation and filtration. Further, adding diluted phosphoric acid solution into the yttrium chloride solution after impurity removal, wherein the byproduct is hydrochloric acid due to the reaction of phosphoric acid and yttrium chloride, and yttrium phosphate is basically dissolved in the hydrochloric acid, so that the precipitation is less, the yttrium phosphate can be directly used as seed crystal, a small amount of ammonia water is added to neutralize a small amount of hydrochloric acid to prepare yttrium phosphate seed crystal, then ammonia water is continuously added, and particles are formed after full reaction, so that yttrium phosphate synthetic solution is obtained; and dehydrating the obtained yttrium phosphate synthetic solution, and adopting a special gradient drying process to obtain yttrium phosphate with purity of more than 99.9%, wherein the iron content is less than 1ppm, and the cobalt, nickel, copper, cadmium, chromium and vanadium content is less than 0.5ppm.
2. The mother liquor in the step 3.1 can be recovered, filtered and evaporated to be concentrated to obtain ammonium chloride crystals which can be used for other purposes, such as chemical fertilizers.
Drawings
FIG. 1 is an XRD pattern of yttrium phosphate prepared in example 1 of the present invention.
Detailed Description
The yttrium phosphate produced in the market is mainly used for fluorescent materials and special ceramics, has low requirements on metal impurities, and is used as an optical glass additive along with the technical development of phosphate optical glass materials. As an optical glass additive, the purity and the metallic impurities (iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like) of the optical glass additive have high index requirements. The preparation process of the yttrium phosphate provided by the invention is simple, the high-purity yttrium phosphate with the content of 99.99% and the content of metal impurities of iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like of less than 0.5ppm can be effectively prepared, and the preparation method of the invention has the advantages of simple industrial operation equipment, mild production condition, extremely low wastewater and waste gas emission and stable and reliable process.
The main reaction equation:
Y2O3+6HCl＝2YCl3+3H2O
YCl3+H3PO4＝YPO4+3HCl
the invention is further described below with reference to the accompanying drawings and specific examples.
Example 1
This example prepares high purity yttrium phosphate by the following steps:
Step 1, purification of yttrium oxide
160Kg of analytically pure hydrochloric acid is added into a reaction kettle, high-purity water is added to dilute the mixture until the mass fraction is 15%, 60kg of yttrium oxide is added into the mixture, the molar ratio of the hydrochloric acid to the yttrium oxide is 6:1, the temperature is raised to 70 ℃, the mixture is stirred and reacts for 30 minutes, the mixture is dissolved to be transparent, the high-purity water is added to dilute the mixture until the specific gravity is 1.11, 60g of metastannic acid (1/1000 of the mass of yttrium oxide) and a small amount of hydrochloric acid (the hydrochloric acid is used for removing iron impurities in yttrium oxide raw materials, the consumption of hydrochloric acid can be estimated according to the content of the iron impurities in the raw materials, the hydrochloric acid can be slightly excessive, ammonia water can be used for neutralization later), after settling for 8 hours, the settled supernatant is filtered through a filter element of 1 micron, and the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like in the supernatant is controlled to be less than 0.1ppm, so that pure yttrium chloride solution is obtained;
step 2, yttrium phosphate synthesis
2.1, Controlling the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like in food-grade phosphoric acid (the mass fraction is 85%) to be less than 0.1ppm, taking 61kg of high-purity water to dilute to 15% by mass fraction, adding the solution into the pure yttrium chloride solution obtained in the step 1, stirring, and heating to 80 ℃;
2.2, controlling the reagent-grade ammonia water until the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like is less than 0.1ppm, adding high-purity water to dilute the reagent-grade ammonia water to 8 mass percent, slowly adding diluted ammonia water with the theoretical mass of 1/10 into the synthetic liquid obtained in the step 2.1, keeping the temperature at 85 ℃ for stirring reaction for 60 minutes to form seed crystals, continuously adding diluted ammonia water to adjust the PH value to 2.5, keeping the temperature at 85 ℃ for stirring reaction for 2 hours, and fully forming particles to obtain yttrium phosphate synthetic liquid;
Step 3, yttrium phosphate dehydration and drying
Step 3.1, pumping the yttrium phosphate synthetic solution into a plate-and-frame filter press, and adopting 1500-mesh filter cloth to carry out filter pressing, washing until the PH is 5 (chloride ions in the mother solution measured at the moment are less than 0.02%), thereby obtaining yttrium phosphate filter cakes;
step 3.2, putting the yttrium phosphate filter cake into a porcelain plate, paving and carrying out gradient drying:
Drying at 250 ℃ for 2 hours in a first gradient;
and (5) drying at 550 ℃ for 3 hours in a second gradient to obtain a target product.
The target product is characterized as yttrium phosphate through xrd, as shown in figure 1.
The content of P 2O5 in the target product is determined to be 38.3% by a quinolylmethylene citrate mixed solution method; the Agilent 5110-ICP-OES detection shows that the cobalt, nickel, titanium, vanadium, chromium, cadmium, copper and lead in the product are all less than 0.5ppm, the iron content is 0.88ppm, and the indexes meet the requirements. The results of the specific assay are shown in the following table:
TABLE 1
Example 2
This example prepares high purity yttrium phosphate by the following steps:
Step 1, purification of yttrium oxide
Adding 212.6kg of analytically pure hydrochloric acid into a reaction kettle, adding high-purity water to dilute to 20% by mass, adding 80kg of yttrium oxide, heating to 70 ℃ and stirring for reaction for 60 minutes, dissolving to be transparent, adding high-purity water to dilute to a specific gravity of 1.12, adding 100g of metastannic acid (1/800 of the mass of yttrium oxide) and a small amount of hydrochloric acid (hydrochloric acid is used for removing iron impurities in yttrium oxide raw materials, the consumption of hydrochloric acid can be estimated according to the content of iron impurities in the raw materials, and ammonia water can be used for neutralization later), filtering the settled supernatant through a 1-micrometer filter element after settling for 8 hours, and controlling the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like in the supernatant to be less than 0.1ppm to obtain a pure yttrium chloride solution;
step 2, yttrium phosphate synthesis
2.1, Controlling the quality of food-grade phosphoric acid (the mass fraction is 85%) to be less than 0.1ppm of iron, cobalt, nickel, copper, cadmium, chromium, vanadium and other elements, taking 81.7kg of high-purity water to dilute to 15% by mass, adding into the yttrium chloride solution obtained in the step 1, stirring, and heating to 70 ℃;
2.2, controlling the reagent-grade ammonia water until the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like is less than 0.1ppm, adding high-purity water to dilute the reagent-grade ammonia water to a mass fraction of 8.5%, slowly adding diluted ammonia water with a theoretical mass of 1/12 into the synthetic liquid obtained in the step 2.1, keeping the temperature at 85 ℃ for stirring and reacting for 45 minutes to form seed crystals, continuously adding diluted ammonia water to adjust the PH value to 3, keeping the temperature at 85 ℃ for stirring and reacting for 2.5 hours, and fully forming particles to obtain yttrium phosphate synthetic liquid;
Step 3, yttrium phosphate dehydration and drying
Step 3.1, pumping the yttrium phosphate synthetic solution into a plate-and-frame filter press, and adopting 1500-mesh filter cloth to carry out filter pressing, washing until the PH is 5.4 (the mass fraction of chloride ions in the mother solution is measured at the moment to be less than 0.02%), thus obtaining yttrium phosphate filter cakes;
step 3.2, putting the yttrium phosphate filter cake into a porcelain plate, paving and carrying out gradient drying:
Drying at 250 ℃ for 3 hours in a first gradient;
and (5) drying at 600 ℃ for 2 hours at the second gradient to obtain the target product.
The target product was identified as yttrium phosphate by xrd, which is substantially identical to that shown in figure 1.
The content of P 2O5 in the target product is determined to be 38.6% by a quinolylmethylene citrate mixed solution method; the Agilent 5110-ICP-OES detection shows that cobalt, nickel, titanium, vanadium, chromium, cadmium, copper and lead in the product are all less than 0.5ppm, iron is 0.92ppm, and the indexes meet the requirements. The results of the specific assay are shown in the following table:
TABLE 2
Example 3
This example prepares high purity yttrium phosphate by the following steps:
Step 1, purification of yttrium oxide
Adding 239.1kg of analytically pure hydrochloric acid into a reaction kettle, adding high-purity water to dilute to 20% by mass, adding 90kg of yttrium oxide, heating to 75 ℃ and stirring for reaction for 60 minutes, dissolving to be transparent, adding high-purity water to dilute to 1.1, adding 180g of metastannic acid (1/500 of the mass of yttrium oxide) and a small amount of hydrochloric acid (the hydrochloric acid is used for removing iron impurities in yttrium oxide raw materials, the consumption of the hydrochloric acid can be estimated according to the iron impurity content in the raw materials, and the raw materials can be neutralized with ammonia water later), filtering the settled supernatant through a 1-micrometer filter element after settling for 8 hours, and controlling the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like in the supernatant to be less than 0.1ppm to obtain a pure yttrium chloride solution;
step 2, yttrium phosphate synthesis
2.1, Controlling the content of iron, cobalt, nickel, copper, cadmium, chromium, vanadium and other elements in food-grade phosphoric acid (the mass fraction is 85%) to be less than 0.1ppm, taking 91.9kg of high-purity water to dilute to 15% by mass fraction, adding the high-purity water into the yttrium chloride solution obtained in the step 1, stirring, and heating to 80 ℃;
2.2, the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like in reagent-grade ammonia water is controlled to be less than 0.1ppm, the ammonia water is diluted to 8 mass percent by adding high-purity water, firstly, the diluted ammonia water with the theoretical mass of 1/10 is slowly added into the synthetic liquid obtained in the step 2.1, the temperature is kept at 85 ℃ and the stirring reaction is carried out for 60 minutes to form seed crystals, then the diluted ammonia water is continuously added to adjust the PH value to 2.7, the temperature is kept at 85 ℃ and the stirring reaction is carried out for 2.5 hours, so that particles are fully formed, and yttrium phosphate synthetic liquid is obtained;
Step 3, yttrium phosphate dehydration and drying
Step 3.1, pumping the yttrium phosphate synthetic solution into a plate-and-frame filter press, and adopting 1500-mesh filter cloth to carry out filter pressing, washing with water until the pH value is 5 (the mass fraction of chloride ions in the mother solution is measured to be less than 0.02 percent at the moment), so as to obtain an yttrium phosphate filter cake;
step 3.2, putting the yttrium phosphate filter cake into a porcelain plate, paving and carrying out gradient drying:
Drying at 280 ℃ for 2.5 hours in a first gradient;
And (5) drying at 550 ℃ for 2 hours in a second gradient to obtain a target product.
The target product was identified as yttrium phosphate by xrd, which is substantially identical to that shown in figure 1.
The content of P 2O5 in the target product is determined to be 38.2% by a quinolylmethylene citrate mixed solution method; the Agilent 5110-ICP-OES detection shows that cobalt, nickel, titanium, vanadium, chromium, cadmium, copper and lead in the product are all less than 0.5ppm, iron is 0.76ppm, and the indexes meet the requirements. The results of the specific assay are shown in the following table:
TABLE 3 Table 3
Example 4
This example prepares high purity yttrium phosphate by the following steps:
Step 1, purification of yttrium oxide
Adding 185.8kg of analytically pure hydrochloric acid into a reaction kettle, adding high-purity water to dilute the solution to 18% by mass, adding 70kg of yttrium oxide into the solution, stirring and reacting the solution for 45 minutes at a temperature of 75 ℃ until the molar ratio of the hydrochloric acid to the yttrium oxide is about 6:1, dissolving the solution until the solution is transparent, adding 100g of metastannic acid (1/700 of the mass of yttrium oxide) and a small amount of hydrochloric acid (the hydrochloric acid is used for removing iron impurities in yttrium oxide raw materials) with a mass fraction of 2.3%, estimating the use amount of the hydrochloric acid according to the iron impurity content in the raw materials, and neutralizing the solution with ammonia water later), filtering the settled supernatant through a 1-micrometer filter element, and controlling the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like in the supernatant to be less than 0.1ppm to obtain a pure yttrium chloride solution after settling for 8 hours;
step 2, yttrium phosphate synthesis
2.1, Controlling the content of iron, cobalt, nickel, copper, cadmium, chromium, vanadium and other elements in food-grade phosphoric acid (the mass fraction is 85%) to be less than 0.1ppm, taking 71.5kg of high-purity water to dilute to 20% by mass fraction, adding the solution into yttrium chloride solution obtained in the step 1, stirring, and heating to 80 ℃;
2.2, controlling the reagent-grade ammonia water until the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like is less than 0.1ppm, adding high-purity water to dilute the reagent-grade ammonia water to 9.5 mass percent, slowly adding diluted ammonia water with the theoretical mass of 1/15 into the synthetic liquid obtained in the step 2.1, keeping the temperature at 90 ℃ for stirring reaction for 30 minutes to form seed crystals, continuously adding diluted ammonia water to adjust the PH value to 3.2, keeping the temperature at 90 ℃ for stirring reaction for 2 hours, and fully forming particles to obtain yttrium phosphate synthetic liquid;
Step 3, yttrium phosphate dehydration and drying
Step 3.1, pumping the yttrium phosphate synthetic solution into a plate-and-frame filter press, and adopting 1500-mesh filter cloth to carry out filter pressing, washing until the PH is 6 (the mass fraction of chloride ions in the mother solution is measured to be less than 0.02%) to obtain an yttrium phosphate filter cake;
step 3.2, putting the yttrium phosphate filter cake into a porcelain plate, paving and carrying out gradient drying:
Drying at 230 ℃ for 2 hours in a first gradient;
and (5) drying for 2 hours at the temperature of 580 ℃ with a second gradient to obtain the target product.
The target product was identified as yttrium phosphate by xrd, which is substantially identical to that shown in figure 1.
The content of P 2O5 in the target product is determined to be 38.4% by a quinolylmethylene citrate mixed solution method; the Agilent 5110-ICP-OES detection shows that cobalt, nickel, titanium, vanadium, chromium, cadmium, copper and lead in the product are all less than 0.5ppm, iron is 0.9ppm, and the indexes meet the requirements. The results of the specific assay are shown in the following table:
TABLE 4 Table 4
Example 5
This example prepares high purity yttrium phosphate by the following steps:
Step 1, purification of yttrium oxide
Adding 239.1kg of analytically pure hydrochloric acid into a reaction kettle, adding high-purity water to dilute to 16% by mass, adding 90kg of yttrium oxide, heating to 72 ℃ and stirring for reaction for 35 minutes, dissolving to be transparent, adding high-purity water to dilute to 1.115, adding 180g of metastannic acid (1/500 of the mass of yttrium oxide) and a small amount of hydrochloric acid (hydrochloric acid is used for removing iron impurities in yttrium oxide raw materials, the consumption of hydrochloric acid can be estimated according to the iron impurity content in the raw materials, and ammonia water can be used for neutralization later), filtering the settled supernatant through a 1-micrometer filter element after settling for 8 hours, and controlling the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like in the supernatant to be less than 0.1ppm to obtain a pure yttrium chloride solution;
step 2, yttrium phosphate synthesis
2.1, Controlling the content of iron, cobalt, nickel, copper, cadmium, chromium, vanadium and other elements in food-grade phosphoric acid (the mass fraction is 85%) to be less than 0.1ppm, taking 91.9kg of high-purity water to dilute to 18%, adding the solution into yttrium chloride solution obtained in the step 1, stirring, and heating to 80 ℃;
2.2, controlling the reagent-grade ammonia water until the content of elements such as iron, cobalt, nickel, copper, cadmium, chromium, vanadium and the like is less than 0.1ppm, adding high-purity water to dilute the reagent-grade ammonia water to 9.5 mass percent, slowly adding diluted ammonia water with the theoretical mass of 1/15 into the synthetic liquid obtained in the step 2.1, keeping the temperature at 90 ℃ for stirring reaction for 30 minutes to form seed crystals, continuously adding diluted ammonia water to adjust the PH value to 3.5, keeping the temperature at 90 ℃ for stirring reaction for 3 hours, and fully forming particles to obtain yttrium phosphate synthetic liquid;
Step 3, yttrium phosphate dehydration and drying
Step 3.1, pumping the yttrium phosphate synthetic solution into a plate-and-frame filter press, and adopting 1500-mesh filter cloth to carry out filter pressing, washing with water until the PH value is 5.6 (the mass fraction of chloride ions in the mother solution is measured at the moment to be less than 0.02 percent), thus obtaining yttrium phosphate filter cakes;
step 3.2, putting the yttrium phosphate filter cake into a porcelain plate, paving and carrying out gradient drying:
drying at 300 ℃ for 2 hours in a first gradient;
and (5) drying at 600 ℃ for 2 hours at the second gradient to obtain the target product.
The target product was identified as yttrium phosphate by xrd, which is substantially identical to that shown in figure 1.
The content of P 2O5 in the target product is determined to be 38.3% by a quinolylmethylene citrate mixed solution method; the Agilent 5110-ICP-OES detection shows that cobalt, nickel, titanium, vanadium, chromium, cadmium, copper and lead in the product are all less than 0.5ppm, iron is 0.85ppm, and the indexes meet the requirements. The results of the specific assay are shown in the following table:
TABLE 5
Claims (6)
1. The preparation method of yttrium phosphate is characterized by comprising the following steps:
Step 1, purifying yttrium oxide
Diluting analytically pure hydrochloric acid to 15-22% by mass fraction with high-purity water, adding yttrium oxide into the solution, heating to 70-75 ℃ and stirring for reaction for 30-60 minutes, dissolving to be transparent, adding high-purity water to dilute to 1.1-1.12, adding metastannic acid and hydrochloric acid with the mass fraction of 1.5-2.5% into the reaction solution, adding 1/500-1/1000 of the mass fraction of the metastannic acid, fully stirring, settling, filtering supernatant, and controlling the contents of iron, cobalt, nickel, copper, cadmium, chromium and vanadium in the supernatant to be less than 0.1ppm to obtain a pure yttrium chloride solution;
step 2, synthesizing yttrium phosphate
Step 2.1, food grade phosphoric acid is centrally controlled until the contents of iron, cobalt, nickel, copper, cadmium, chromium and vanadium are all less than 0.1ppm, water is added for dilution until the mass fraction is 15-20%, the mixture is added into yttrium chloride solution, and the mixture is stirred and heated to 70-80 ℃;
2.2, the reagent grade ammonia water is centrally controlled until the iron, cobalt, nickel, copper, cadmium, chromium and vanadium contents are less than 0.1ppm, the reagent grade ammonia water is diluted by adding high-purity water until the mass fraction is 8-9.5%, firstly, diluted ammonia water with the theoretical mass of 1/10-1/15 is added into the synthetic liquid in the step 2.1, the temperature is kept at 85-90 ℃ for stirring reaction for 30-60 minutes to form seed crystals, then, diluted ammonia water is continuously added into the synthetic liquid, the PH value is adjusted to 2.5-3.5, the temperature is kept at 85-90 ℃ for stirring reaction for 2-3 hours, and the particles are fully formed to obtain yttrium phosphate synthetic liquid;
Step 3, dehydrating and drying yttrium phosphate
Step 3.1, press-filtering the yttrium phosphate synthetic liquid, and then washing until the PH is 5-6 to obtain a yttrium phosphate filter cake;
step 3.2, carrying out gradient drying on the yttrium phosphate filter cake:
a first gradient: drying at 200-300 deg.c for 2-3 hr;
a second gradient: drying at 500-600 deg.c for 2-3 hr to obtain high purity yttrium phosphate.
2. The method for preparing yttrium phosphate according to claim 1, wherein: in step 1, high purity water is added to dilute the mixture to a specific gravity of 1.1.
3. The method for preparing yttrium phosphate according to claim 2, wherein: in step 2.2, the pH is adjusted to 2.7.
4. A method of preparing yttrium phosphate according to claim 3, wherein: the step 3.1 specifically comprises the following steps: pumping the yttrium phosphate synthetic solution into a plate-and-frame filter press, and adopting filter cloth with more than 1500 meshes to filter-press, washing with water until the PH is 5-6, thus obtaining yttrium phosphate filter cakes.
5. A high purity yttrium phosphate, characterized in that: prepared by the method of any one of claims 1-4.
6. An optical glass, characterized in that: the high purity yttrium phosphate of claim 5 is added during glass melting.
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