CN114349481A - Buoyancy material capable of resisting temperature of 1500 ℃ and preparation method thereof - Google Patents
Buoyancy material capable of resisting temperature of 1500 ℃ and preparation method thereof Download PDFInfo
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- CN114349481A CN114349481A CN202111433198.9A CN202111433198A CN114349481A CN 114349481 A CN114349481 A CN 114349481A CN 202111433198 A CN202111433198 A CN 202111433198A CN 114349481 A CN114349481 A CN 114349481A
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- 239000000463 material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 81
- 238000001035 drying Methods 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 238000001816 cooling Methods 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001354 calcination Methods 0.000 claims abstract description 14
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 239000011499 joint compound Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 9
- 239000006184 cosolvent Substances 0.000 claims abstract description 9
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 9
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000835 fiber Substances 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 9
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 33
- 239000002245 particle Substances 0.000 claims description 20
- 238000000034 method Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 3
- 239000002694 phosphate binding agent Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 239000011230 binding agent Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention provides a buoyancy material capable of resisting temperature of 1500 ℃ and a preparation method thereof, and the buoyancy material comprises the following steps: (1) respectively cleaning the alumina hollow spheres by using distilled water, and then drying; (2) uniformly mixing according to the mass ratio of 2:1: 2; (3) uniformly mixing the alumina hollow spheres with 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1; (4) then adding spherical silicon dioxide powder, a boron oxide cosolvent and chopped mullite fiber, and uniformly mixing; (5) molding the mixture obtained in the step (4) in a six-joint cement rapid test mold; (6) drying and curing the formed sample; (7) and cooling the cured sample at room temperature, demolding, calcining, and naturally cooling to obtain the buoyancy material with the temperature resistance of 1500 ℃.
Description
Technical Field
The invention belongs to the technical field of marine buoyancy materials, and particularly relates to a 1500 ℃ high-temperature-resistant buoyancy material and a preparation method thereof.
Background
According to the depth of seawater, the international oceanographic community refers to the depth of 6000-11000 meters as "deep Yuan". Marine life, marine ecology, submarine geology and the like in the deep-brillouin area play an important role in the research of earth ecology, climate, life origin, earthquake prediction and the like.
Deep sea resource development, ocean expansion living space and ocean military field, which all put strong requirements on the temperature resistance of the buoyancy material. At present, the buoyancy material adopted at home and abroad is mainly a resin-based organic solid buoyancy material and is composed of an organic resin matrix and hollow ceramic microspheres. Although the hollow ceramic microspheres have certain temperature resistance, the resin matrix does not resist high temperature, so the temperature resistance of the buoyancy material depends on the matrix of the buoyancy material.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a buoyancy material capable of resisting 1500 ℃ and a preparation method thereof, and the prepared buoyancy material has high temperature resistance and compression resistance and can be used as an inorganic buoyancy material capable of resisting 1500 ℃.
In order to solve the technical problem, the invention provides the following technical scheme:
a preparation method of a buoyancy material capable of resisting temperature of 1500 ℃ comprises the following steps:
(1) respectively cleaning alumina hollow spheres with the particle sizes of 0.50mm,1.00mm and 2.00mm by using distilled water, then placing the alumina hollow spheres into an oven, and drying the alumina hollow spheres for 4 hours at 70 ℃;
(2) drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the mass ratio of 2:1: 2;
(3) uniformly mixing the uniformly mixed alumina hollow spheres and 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1;
(4) then adding spherical silicon dioxide powder accounting for 30-50% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 0-6% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 0-12% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture obtained in the step (4) into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, continuously heating to 1500 ℃, preserving heat for 4h, calcining, and naturally cooling to obtain the buoyancy material capable of resisting 1500 ℃.
Preferably, the aluminum dihydrogen phosphate solution with the concentration of 98% is an aluminum dihydrogen phosphate solution with the concentration of 98%.
Optimally, the six-joint cement rapid test model specification is 20 multiplied by 20 mm.
Preferably, in the step (7), the heating rate during the calcination is 5 ℃/min.
A buoyancy material capable of resisting 1500 ℃, which is prepared by the following steps:
(1) respectively cleaning alumina hollow spheres with the particle sizes of 0.50mm,1.00mm and 2.00mm by using distilled water, placing the alumina hollow spheres into an oven, and drying the alumina hollow spheres for 4 hours at 70 ℃;
(2) drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2;
(3) uniformly mixing the uniformly mixed alumina hollow spheres and 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1;
(4) then adding spherical silicon dioxide powder accounting for 40% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 4% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 8% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, keeping the temperature for 4h, calcining, and naturally cooling to obtain the 1500-DEG C-resistant buoyancy material.
The aluminum dihydrogen phosphate solution with the concentration of 98% and the spherical silicon dioxide powder binding agent are used as high-temperature binding agents to be combined with the alumina hollow sphere buoyancy material, obvious plastic deformation does not occur at 1500 ℃, the temperature resistance and the compression resistance are high, and the aluminum dihydrogen phosphate solution can be used as an inorganic buoyancy material with the temperature resistance of 1500 ℃.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a buoyancy material capable of resisting 1500 ℃, which is prepared by the following steps:
(1) respectively cleaning alumina hollow spheres with the particle sizes of 0.50mm,1.00mm and 2.00mm by using distilled water, placing the alumina hollow spheres into an oven, and drying the alumina hollow spheres for 4 hours at 70 ℃;
(2) drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2;
(3) uniformly mixing the uniformly mixed alumina hollow spheres and 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1;
(4) then adding spherical silicon dioxide powder accounting for 40% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 4% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 8% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, keeping the temperature for 4h, calcining, and naturally cooling to obtain the 1500-DEG C-resistant buoyancy material.
The buoyancy material obtained by the embodiment has no obvious plastic deformation at 1500 ℃, has high temperature resistance and high compression resistance, and can be used as an inorganic buoyancy material with 1500 ℃.
Example 2:
a buoyancy material capable of resisting 1500 ℃, which is prepared by the following steps:
(1) respectively cleaning alumina hollow spheres with particle sizes of 0.50mm,1.00mm and 2.00mm with distilled water, placing in an oven, and drying at 70 deg.C for 4 h.
(2) And drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2.
(3) And uniformly mixing the uniformly mixed alumina hollow spheres and 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1.
(4) Then, spherical silica powder accounting for 30 percent of the mass of the alumina hollow sphere is added and mixed evenly.
(5) The mixture was poured into a 20X 20mm six-pack cement rapid test mold and shaped.
(6) And (3) preserving the temperature of the formed sample in an oven at 70 ℃ for 24h, and drying and curing.
(7) And cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, and carrying out heat preservation for 4 hours.
Step (7) comparing with test 1, cooling the solidified sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1400 ℃, and carrying out calcination treatment for heat preservation for 4 hours; and (7) comparing with the test 2, cooling the solidified sample at room temperature, demolding, placing the cooled sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1400 ℃, and carrying out heat preservation for 4 hours.
The following are found: in this example, under otherwise identical conditions, the compressive strength of the obtained buoyancy material was the strongest when calcination was performed at 1500 ℃.
Example 3:
a buoyancy material capable of resisting 1500 ℃, which is prepared by the following steps:
1) respectively cleaning alumina hollow spheres with particle sizes of 0.50mm,1.00mm and 2.00mm with distilled water, placing in an oven, and drying at 70 deg.C for 4 h.
(2) And drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2.
(3) And uniformly mixing the uniformly mixed alumina hollow spheres and 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1.
(4) Then, spherical silica powder accounting for 40% of the mass fraction of the alumina hollow spheres is added and mixed uniformly.
(5) The mixture was poured into a 20X 20mm six-pack cement rapid test mold and shaped.
(6) And (3) preserving the temperature of the formed sample in an oven at 70 ℃ for 24h, and drying and curing.
(7) And cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, and carrying out heat preservation for 4 hours.
Step (4) control test: adding spherical silicon dioxide powder accounting for 50% of the mass fraction of the alumina hollow spheres.
The following are found: when the mass fraction of the spherical silicon dioxide powder relative to the alumina hollow sphere is 40%, the volume density of the obtained buoyancy material is 1.30g/cm at least3And the compressive strength of the sample is not obviously changed by 3.01MPa along with the content of the spherical silicon dioxide powder. Taking the physical properties of the samples of examples 2 and 3 into account, the amount of spherical silica powder added was selected to be 40wt.% and the calcination temperature was 1500 ℃.
Example 4:
a buoyancy material capable of resisting 1500 ℃, which is prepared by the following steps:
1) respectively cleaning alumina hollow spheres with particle sizes of 0.50mm,1.00mm and 2.00mm with distilled water, placing in an oven, and drying at 70 deg.C for 4 h.
(2) And drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2.
(3) And uniformly mixing the uniformly mixed alumina hollow spheres and a phosphate binder according to the mass ratio of 2: 1.
(4) Then adding spherical silicon dioxide powder accounting for 40% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 4% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 4% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, keeping the temperature for 4h, calcining, and naturally cooling to obtain the 1500-DEG C-resistant buoyancy material.
The buoyancy material obtained by the embodiment has no obvious plastic deformation at 1500 ℃, and has high temperature resistance and high compression resistance.
Example 5:
a buoyancy material capable of resisting 1500 ℃, which is prepared by the following steps:
1) respectively cleaning alumina hollow spheres with particle sizes of 0.50mm,1.00mm and 2.00mm with distilled water, placing in an oven, and drying at 70 deg.C for 4 h.
(2) And drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2.
(3) And uniformly mixing the uniformly mixed alumina hollow spheres and a phosphate binder according to the mass ratio of 2: 1.
(4) Then adding spherical silicon dioxide powder accounting for 40% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 6% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 8% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, keeping the temperature for 4h, calcining, and naturally cooling to obtain the 1500-DEG C-resistant buoyancy material.
The buoyancy material obtained by the embodiment has no obvious plastic deformation at 1500 ℃, and has high temperature resistance and high compression resistance.
Example 6:
a buoyancy material capable of resisting 1500 ℃, which is prepared by the following steps:
1) respectively cleaning alumina hollow spheres with particle sizes of 0.50mm,1.00mm and 2.00mm with distilled water, placing in an oven, and drying at 70 deg.C for 4 h.
(2) And drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2.
(3) And uniformly mixing the uniformly mixed alumina hollow spheres and a phosphate binder according to the mass ratio of 2: 1.
(4) Then adding spherical silicon dioxide powder accounting for 40% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 2% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 12% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, keeping the temperature for 4h, calcining, and naturally cooling to obtain the 1500-DEG C-resistant buoyancy material.
The buoyancy material obtained by the embodiment has no obvious plastic deformation at 1500 ℃, and has high temperature resistance and high compression resistance.
Claims (5)
1. A preparation method of a buoyancy material capable of resisting temperature of 1500 ℃ is characterized by comprising the following steps: comprises the following steps:
(1) respectively cleaning alumina hollow spheres with the particle sizes of 0.50mm,1.00mm and 2.00mm by using distilled water, then placing the alumina hollow spheres into an oven, and drying the alumina hollow spheres for 4 hours at 70 ℃;
(2) drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the mass ratio of 2:1: 2;
(3) uniformly mixing the uniformly mixed alumina hollow spheres and 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1;
(4) then adding spherical silicon dioxide powder accounting for 30-50% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 0-6% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 0-12% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture obtained in the step (4) into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, continuously heating to 1500 ℃, preserving heat for 4h, calcining, and naturally cooling to obtain the buoyancy material capable of resisting 1500 ℃.
2. The method of claim 1, wherein: the aluminum dihydrogen phosphate solution with the concentration of 98 percent is an aluminum dihydrogen phosphate solution with the concentration of 98 percent.
3. The method of claim 2, wherein: the six-joint cement rapid test specification is 20 multiplied by 20 mm.
4. The production method according to claim 3, characterized in that: in the step (7), the temperature rise rate during calcination is 5 ℃/min.
5. The buoyancy material capable of resisting temperature of 1500 ℃ is characterized in that: the buoyancy material is prepared by the following steps:
(1) respectively cleaning alumina hollow spheres with the particle sizes of 0.50mm,1.00mm and 2.00mm by using distilled water, placing the alumina hollow spheres into an oven, and drying the alumina hollow spheres for 4 hours at 70 ℃;
(2) drying the three alumina hollow spheres with the particle sizes, and uniformly mixing the dried three alumina hollow spheres according to the ratio of 2:1: 2;
(3) uniformly mixing the uniformly mixed alumina hollow spheres and 98% aluminum dihydrogen phosphate solution according to the mass ratio of 2: 1;
(4) then adding spherical silicon dioxide powder accounting for 40% of the mass fraction of the alumina hollow spheres, a boron oxide cosolvent accounting for 4% of the mass fraction of the alumina hollow spheres and chopped mullite fiber accounting for 8% of the mass fraction of the alumina hollow spheres, and uniformly mixing;
(5) pouring the mixture into a six-joint cement rapid test mold with the size of 20 multiplied by 20mm for molding;
(6) keeping the formed sample in an oven at 70 ℃ for 24h, and drying and curing;
(7) and cooling the cured sample at room temperature, demolding, placing the sample in a high-temperature furnace, heating at the heating rate of 5 ℃/min, continuously heating to 1500 ℃, keeping the temperature for 4h, calcining, and naturally cooling to obtain the 1500-DEG C-resistant buoyancy material.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948791A (en) * | 2016-05-04 | 2016-09-21 | 山东理工大学 | Preparation method for preparing lightweight and porous aluminium phosphate-alumina ceramic ball |
| CN109694240A (en) * | 2017-10-24 | 2019-04-30 | 天津大学（青岛）海洋工程研究院有限公司 | A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material |
| CN110498673A (en) * | 2019-07-31 | 2019-11-26 | 辽宁科技大学 | A kind of mullite crystal whisker enhancing alumina hollow ball porous ceramics preparation method |
-
2021
- 2021-11-29 CN CN202111433198.9A patent/CN114349481A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948791A (en) * | 2016-05-04 | 2016-09-21 | 山东理工大学 | Preparation method for preparing lightweight and porous aluminium phosphate-alumina ceramic ball |
| CN109694240A (en) * | 2017-10-24 | 2019-04-30 | 天津大学（青岛）海洋工程研究院有限公司 | A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material |
| CN110498673A (en) * | 2019-07-31 | 2019-11-26 | 辽宁科技大学 | A kind of mullite crystal whisker enhancing alumina hollow ball porous ceramics preparation method |
Non-Patent Citations (1)
| Title |
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| 耿海涛: "中空陶瓷微球基无机固体浮力材料的制备与性能研究", 《中国博士学位论文全文数据库·工程科技Ⅰ辑》 * |
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Application publication date: 20220415 |