Low-zirconium high-whiteness synthetic zirconium material and preparation method thereof

Abstract

The preparation method comprises the following steps: S1, preparing a zirconium oxide precursor: mixing carbonate and ammonium nitrate according to a certain proportion, adding a proper amount of water, uniformly stirring, heating to 80 DEG C or above to obtain an oxide precipitate, and then drying, screening and the like the precipitate to obtain the zirconium oxide precursor; obtaining a zirconium oxide precursor; s2, preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then dropwise adding into ethanol to obtain the rare earth element additive; s3, preparing a synthetic zirconium material: uniformly mixing the zirconium oxide precursor, alkali carbonate and a rare earth element additive according to a certain proportion, then adding a proper amount of water, mechanically stirring, finally putting the mixture into a high-temperature furnace, and calcining under the protection of atmosphere to obtain the low-zirconium high-whiteness synthetic zirconium material.

Description

Technical Field

[0001] The invention relates to the technical field of zirconium materials, in particular to a low-zirconium and high-white synthetic zirconium material and a preparation method thereof. Background Art

[0002] In the traditional zirconium material preparation process, natural ores containing a large amount of impurities such as zircon are usually used as raw materials, resulting in the prepared zirconium materials having a high impurity content and relative density. In addition, the preparation process of zirconium materials often requires high temperature and high pressure conditions, which not only increases energy consumption and production costs, but also affects the physical and chemical properties of the materials.

[0003] Therefore, developing a low-zirconium and high-white synthetic zirconium material and a preparation method thereof can not only reduce the preparation cost of the material, but also improve the quality and stability of the material, and has important application value. Summary of the invention

[0004] The object of the present invention is to provide a low-zirconium and high-white synthetic zirconium material and a preparation method thereof, which has the advantages of environmental protection, low production cost and stable quality of the synthetic zirconium material.

[0005] To achieve the above object, the present invention provides the following technical solution: a low-zirconium and high-white synthetic zirconium material, comprising the following components by weight:

[0006] Zirconia 85-95%;

[0007] Alkali metal carbonate 5-15%;

[0008] Rare earth element additive 0.1-2%.

[0009] The components by weight include the following:

[0010] Zirconia 88-92%;

[0011] Alkali metal carbonates 7-12%;

[0012] Rare earth element additive 0.2-1.5%.

[0013] A method for preparing a low-zirconium and high-white synthetic zirconium material, characterized in that it comprises the following steps:

[0014] S1: preparing a zirconium oxide precursor: mixing carbonate and ammonium nitrate in a certain proportion, adding an appropriate amount of water, stirring evenly, and heating to above 80° C. to obtain an oxide precipitate, and then drying and sieving the precipitate to obtain a zirconium oxide precursor;

[0015] S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive;

[0016] S3 Preparation of synthetic zirconium material: The zirconium oxide precursor, alkali metal carbonate and rare earth element additive are mixed evenly in a certain proportion, and then an appropriate amount of water is added and mechanically stirred. Finally, the mixture is placed in a high-temperature furnace and calcined under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material.

[0017] Preferably, in step S1, the ratio of carbonate to ammonium nitrate is 1:1 or 1:2.

[0018] Preferably, in step S1, the prepared precipitate is washed multiple times with deionized water to remove unnecessary ions and impurities, and a centrifuge or a vacuum filter can be used for washing.

[0019] Preferably, in step S1, the washed precipitate is filtered and placed in a glass apparatus, and is dried in an oven, usually at a temperature of 80-120° C. for 4 hours, until completely dried.

[0020] Preferably, in step S1, the precipitate after drying forms a granular solid, which needs to be sieved using a sieve to remove oversized or undersized particles, and the mesh size of the sieve is 200-400 meshes.

[0021] Preferably, in step S3, the calcination time is 2-10 hours, and the calcination temperature is 1300-1800°C.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] The invention adopts inorganic materials such as zirconium oxide, alkali metal carbonate and rare earth elements, and has good environmental protection. High temperature and high pressure conditions are not required in the preparation process, which reduces production costs and energy consumption. The prepared synthetic zirconium material has stable quality, high whiteness and low zirconium content, and is suitable for application in various fields. DETAILED DESCRIPTION

[0024] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0025] Embodiment 1:

[0026] A low-zirconium and high-white synthetic zirconium material, comprising the following components:

[0027] Zirconia 88%;

[0028] Alkali metal carbonates 10.8%;

[0029] Rare earth element additive 1.2%.

[0030] A method for preparing a low-zirconium and high-white synthetic zirconium material comprises the following steps:

[0031] S1 Preparation of zirconium oxide precursor: Mix carbonate and ammonium nitrate in a certain proportion, add appropriate amount of water, stir evenly, and heat to above 80°C to obtain an oxide precipitate. Then, the precipitate is dried, sifted and processed to obtain a zirconium oxide precursor. The ratio of carbonate and ammonium nitrate is 1:1. The prepared precipitate is washed with deionized water for multiple times to remove unnecessary ions and impurities. A centrifuge or vacuum filter can be used for washing. The washed precipitate is filtered and placed in a glass instrument. It is dried in an oven, usually at a temperature of 80°C for 4 hours, until completely dry. The dried precipitate will form a granular solid, which needs to be sieved with a sieve to remove particles that are too large or too small. The mesh size of the sieve is 300 mesh.

[0032] S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive;

[0033] S3 Preparation of synthetic zirconium material: Mix the zirconium oxide precursor, alkali metal carbonate and rare earth element additives in a certain proportion, then add an appropriate amount of water and stir mechanically. Finally, place the mixture in a high-temperature furnace and calcine it under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material. The calcination time is 5 hours and the calcination temperature is 1400°C.

[0034] Embodiment 2:

[0035] A low-zirconium and high-white synthetic zirconium material, comprising the following components:

[0036] Zirconia 88%;

[0037] Alkali metal carbonate 11%;

[0038] Rare earth element additive 1%.

[0039] A method for preparing a low-zirconium and high-white synthetic zirconium material comprises the following steps:

[0040] S1 Preparation of zirconium oxide precursor: Mix carbonate and ammonium nitrate in a certain proportion, add appropriate amount of water, stir evenly, and heat to above 80°C to obtain an oxide precipitate. Then, the precipitate is dried, sifted and processed to obtain a zirconium oxide precursor. The ratio of carbonate and ammonium nitrate is 1:1. The prepared precipitate is washed with deionized water for multiple times to remove unnecessary ions and impurities. A centrifuge or vacuum filter can be used for washing. The washed precipitate is filtered and placed in a glass instrument. It is dried in an oven, usually at a temperature of 80°C for 4 hours, until completely dry. The dried precipitate will form a granular solid, which needs to be sieved with a sieve to remove particles that are too large or too small. The mesh size of the sieve is 300 mesh.

[0041] S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive;

[0042] S3 Preparation of synthetic zirconium material: Mix the zirconium oxide precursor, alkali metal carbonate and rare earth element additives in a certain proportion, then add an appropriate amount of water and stir mechanically. Finally, place the mixture in a high-temperature furnace and calcine it under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material. The calcination time is 5 hours and the calcination temperature is 1400°C.

[0043] Embodiment three:

[0044] A low-zirconium and high-white synthetic zirconium material, comprising the following components:

[0045] Zirconia 88%;

[0046] Alkali metal carbonates 11.5%;

[0047] Rare earth element additive 0.5%.

[0048] A method for preparing a low-zirconium and high-white synthetic zirconium material comprises the following steps:

[0049] S1 Preparation of zirconium oxide precursor: Mix carbonate and ammonium nitrate in a certain proportion, add appropriate amount of water, stir evenly, and heat to above 80°C to obtain an oxide precipitate. Then, the precipitate is dried, sifted and processed to obtain a zirconium oxide precursor. The ratio of carbonate and ammonium nitrate is 1:1. The prepared precipitate is washed with deionized water for multiple times to remove unnecessary ions and impurities. A centrifuge or vacuum filter can be used for washing. The washed precipitate is filtered and placed in a glass instrument. It is dried in an oven, usually at a temperature of 80°C for 4 hours, until completely dry. The dried precipitate will form a granular solid, which needs to be sieved with a sieve to remove particles that are too large or too small. The mesh size of the sieve is 300 mesh.

[0050] S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive;

[0051] S3 Preparation of synthetic zirconium material: Mix the zirconium oxide precursor, alkali metal carbonate and rare earth element additives in a certain proportion, then add an appropriate amount of water and stir mechanically. Finally, place the mixture in a high-temperature furnace and calcine it under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material. The calcination time is 5 hours and the calcination temperature is 1400°C.

[0052] Embodiment 4:

[0053] A low-zirconium and high-white synthetic zirconium material, comprising the following components:

[0054] Zirconia 88%;

[0055] Alkali metal carbonates 10.8%;

[0056] Rare earth element additive 1.2%.

[0057] A method for preparing a low-zirconium and high-white synthetic zirconium material comprises the following steps:

[0058] S1 Preparation of zirconium oxide precursor: Mix carbonate and ammonium nitrate in a certain proportion, add appropriate amount of water, stir evenly, and heat to above 80°C to obtain an oxide precipitate. Then, the precipitate is dried, sifted and processed to obtain a zirconium oxide precursor. The ratio of carbonate and ammonium nitrate is 1:2. The prepared precipitate is washed with deionized water for multiple times to remove unnecessary ions and impurities. A centrifuge or vacuum filter can be used for washing. The washed precipitate is filtered and placed in a glass instrument. It is dried in an oven, usually at a temperature of 80°C for 4 hours, until completely dried. The dried precipitate will form a granular solid, which needs to be sieved with a sieve to remove particles that are too large or too small. The mesh size of the sieve is 300 mesh.

[0059] S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive;

[0060] S3 Preparation of synthetic zirconium material: Mix the zirconium oxide precursor, alkali metal carbonate and rare earth element additives in a certain proportion, then add an appropriate amount of water and stir mechanically. Finally, place the mixture in a high-temperature furnace and calcine it under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material. The calcination time is 5 hours and the calcination temperature is 1400°C.

[0061] Embodiment five:

[0062] A low-zirconium and high-white synthetic zirconium material, comprising the following components:

[0063] Zirconia 88%;

[0064] Alkali metal carbonate 11%;

[0065] Rare earth element additive 1%.

[0066] A method for preparing a low-zirconium and high-white synthetic zirconium material comprises the following steps:

[0067] S1 Preparation of zirconium oxide precursor: Mix carbonate and ammonium nitrate in a certain proportion, add appropriate amount of water, stir evenly, and heat to above 80°C to obtain an oxide precipitate. Then, the precipitate is dried, sifted and processed to obtain a zirconium oxide precursor. The ratio of carbonate and ammonium nitrate is 1:2. The prepared precipitate is washed with deionized water for multiple times to remove unnecessary ions and impurities. A centrifuge or vacuum filter can be used for washing. The washed precipitate is filtered and placed in a glass instrument. It is dried in an oven, usually at a temperature of 80°C for 4 hours, until completely dried. The dried precipitate will form a granular solid, which needs to be sieved with a sieve to remove particles that are too large or too small. The mesh size of the sieve is 300 mesh.

[0068] S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive;

[0069] S3 Preparation of synthetic zirconium material: Mix the zirconium oxide precursor, alkali metal carbonate and rare earth element additives in a certain proportion, then add an appropriate amount of water and stir mechanically. Finally, place the mixture in a high-temperature furnace and calcine it under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material. The calcination time is 5 hours and the calcination temperature is 1400°C.

[0070] Embodiment six:

[0071] A low-zirconium and high-white synthetic zirconium material, comprising the following components:

[0072] Zirconia 88%;

[0073] Alkali metal carbonates 11.5%;

[0074] Rare earth element additive 0.5%.

[0075] A method for preparing a low-zirconium and high-white synthetic zirconium material comprises the following steps:

[0076] S1 Preparation of zirconium oxide precursor: Mix carbonate and ammonium nitrate in a certain proportion, add appropriate amount of water, stir evenly, and heat to above 80°C to obtain an oxide precipitate. Then, the precipitate is dried, sifted and processed to obtain a zirconium oxide precursor. The ratio of carbonate and ammonium nitrate is 1:2. The prepared precipitate is washed with deionized water for multiple times to remove unnecessary ions and impurities. A centrifuge or vacuum filter can be used for washing. The washed precipitate is filtered and placed in a glass instrument. It is dried in an oven, usually at a temperature of 80°C for 4 hours, until completely dried. The dried precipitate will form a granular solid, which needs to be sieved with a sieve to remove particles that are too large or too small. The mesh size of the sieve is 300 mesh.

[0077] S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive;

[0078] S3 Preparation of synthetic zirconium material: Mix the zirconium oxide precursor, alkali metal carbonate and rare earth element additives in a certain proportion, then add an appropriate amount of water and stir mechanically. Finally, place the mixture in a high-temperature furnace and calcine it under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material. The calcination time is 5 hours and the calcination temperature is 1400°C.

[0079] Mechanical properties test

[0080] The tensile strength test of the materials prepared in Example 1, Example 2, Example 3, Example 4, Example 5 and Example 6 was performed using a universal testing machine. The test results are shown in Table 1:

[0081] Sample name Tensile strength(Mpa) Embodiment 1 710 Embodiment 2 720 Embodiment 3 750 Embodiment 4 730 Embodiment 5 750 Embodiment 6 780

[0082] In Example 1, Example 2, Example 3, Example 4, Example 5 and Example 6, the calcination temperature in step S3 is changed from 1400°C to 1500°C, 1500°C to 1600°C, 1600°C to 1700°C, and 1700°C to 1800°C, and the four intervals are prepared respectively. The prepared materials are respectively subjected to tensile strength tests, and the results are shown in Table 2 (1400°C-1500°C):

[0083]

[0084]

[0085] Table 3 (1500℃-1600℃)

[0086] Sample name Tensile strength(Mpa) Embodiment 1 730 Embodiment 2 740 Embodiment 3 770 Embodiment 4 750 Embodiment 5 770 Embodiment 6 800

[0087] Table 4 (1600℃-1700℃)

[0088] Sample name Tensile strength(Mpa) Embodiment 1 725 Embodiment 2 735 Embodiment 3 760 Embodiment 4 740 Embodiment 5 760 Embodiment 6 785

[0089] Table 5 (1700℃-1800℃)

[0090] Sample name Tensile strength(Mpa) Embodiment 1 705 Embodiment 2 715 Embodiment 3 720 Embodiment 4 710 Embodiment 5 720 Embodiment 6 725

[0091] From the data in Table 1, Table 2, Table 3, Table 4 and Table 5, we know that:

[0092] (1) In Table 1, the difference between Example 1, Example 2 and Example 3 and Example 4, Example 5 and Example 6 lies in the ratio of carbonate to ammonium nitrate. From the test results, it is known that when the ratio of carbonate to ammonium nitrate is 1:2, the tensile strength of the material prepared in Example 6 is higher;

[0093] (2) In Table 1, it is known from the test results of Example 4, Example 5 and Example 6 that the content of alkali metal carbonate plays an important role in the research and development of low-zirconium and high-white synthetic zirconium materials. The higher the content, the higher the tensile strength.

[0094] (3) From the data in Tables 2, 3, 4 and 5, it can be seen that after changing the calcination temperature, the tensile strength of the low-zirconium high-white synthetic zirconium material also changes accordingly. In the calcination temperature range of 1500℃-1600℃, the tensile strength of the low-zirconium high-white synthetic zirconium material is the highest, which can reach 800Mpa.

[0095] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0096] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A low-zirconium and high-white synthetic zirconium material, characterized in that: The components by weight include the following: Zirconia 85-95%; Alkali metal carbonate 5-15%; Rare earth element additive 0.1-2%.

2. A low-zirconium and high-white synthetic zirconium material according to claim 1, characterized in that: The components by weight include the following: Zirconia 88-92%; Alkali metal carbonates 7-12%; Rare earth element additive 0.2-1.5%.

3. A method for preparing a low-zirconium and high-white synthetic zirconium material, characterized in that: The following steps are involved: S1: preparing a zirconium oxide precursor: mixing carbonate and ammonium nitrate in a certain proportion, adding an appropriate amount of water, stirring evenly, and heating to above 80° C. to obtain an oxide precipitate, and then drying and sieving the precipitate to obtain a zirconium oxide precursor; S2: preparing a rare earth element additive: dissolving a rare earth element compound in a small amount of dilute acid, and then adding the acid dropwise into ethanol to obtain a rare earth element additive; S3 Preparation of synthetic zirconium material: The zirconium oxide precursor, alkali metal carbonate and rare earth element additive are mixed evenly in a certain proportion, and then an appropriate amount of water is added and mechanically stirred. Finally, the mixture is placed in a high-temperature furnace and calcined under atmosphere protection to obtain a low-zirconium and high-white synthetic zirconium material.

4. The method for preparing a low-zirconium and high-white synthetic zirconium material according to claim 3, characterized in that: In step S1, the ratio of carbonate to ammonium nitrate is 1:1 or 1:

2.

5. The method for preparing a low-zirconium and high-white synthetic zirconium material according to claim 3, characterized in that: In step S1, the prepared precipitate is washed multiple times with deionized water to remove unnecessary ions and impurities. A centrifuge or a vacuum filter may be used for washing.

6. The method for preparing a low-zirconium and high-white synthetic zirconium material according to claim 3, characterized in that: In the step S1, the washed precipitate is filtered and placed in a glass apparatus, and is dried in an oven, usually at a temperature of 80-120° C. for 4 hours, until it is completely dried.

7. The method for preparing a low-zirconium and high-white synthetic zirconium material according to claim 3, characterized in that: In the step S1, the precipitate after drying will form a granular solid, which needs to be screened using a sieve to remove oversized or undersized particles. The mesh size of the sieve is 200-400 meshes.

8. The method for preparing a low-zirconium and high-white synthetic zirconium material according to claim 3, characterized in that: In step S3, the calcination time is 2-10 hours, and the calcination temperature is 1300-1800°C.

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