CN109694240A - A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material - Google Patents
A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material Download PDFInfo
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- CN109694240A CN109694240A CN201711004193.8A CN201711004193A CN109694240A CN 109694240 A CN109694240 A CN 109694240A CN 201711004193 A CN201711004193 A CN 201711004193A CN 109694240 A CN109694240 A CN 109694240A
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- floating bead
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- mullite
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- buoyancy material
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/606—Drying
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/95—Products characterised by their size, e.g. microceramics
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Abstract
A kind of high temperature resistant floating bead/mullite solid buoyancy material preparation method, comprising: the pretreatment of floating bead, the preparation of premixed liquid, the preparation of floating bead/mullite slurry, the preparation of floating bead/mullite buoyant material；Material compression strength with higher, preferable temperature tolerance and higher high temperature compression strength, simple process, experiment is easy to operate, and prepared material normal temperature compressed intensity with higher and high temperature compression strength provide possibility in deep-sea for potential demand.
Description
Technical field
The invention belongs to structural material preparation technical field, in particular to a kind of high temperature resistant floating bead/mullite solid buoyancy
The preparation method of material.
Background technique
With economic continuous development, the mankind constantly excessively develop natural resources, and land resources are used as to be distributed in the world
Most wide, the maximum resource of quantity, has been far from satisfying the growing material requisite of the mankind.Ocean as the mankind or
The direction that emphasis in future is explored, contains abundant mineral resources, and Ocean energy resource is the long term growth in the world
A reliable material guarantee is provided, construction and Development of Marine become the inexorable trend of current social development.Currently, deep-sea is opened
Hair can be observed in deep-sea field using benthoscope, be measured, being sampled, install must mainly based on deep submergence technology
Instrument wanted etc. carries out underwater operation.It can not be reached in deep-sea in the mankind, various detected events will then be assisted by underwater robot
To complete.Judging from the current situation, benthoscope, especially deep sea manned submersible are the emphasis of ocean development.
During exploration, the mankind will also be faced with huge difficult and challenge, in addition to will be by deep-sea
Outside huge pressure, i.e., every depth for increasing 100m, the pressure that object is subject to just will increase about 10 atmospheric pressure, i.e. 1MPa.This
Outside, material property is also possible to will receive the influence of particular surroundings.It is past when launching a guided missile in deep-sea as torpedo, anti-warship guided missle etc.
Toward that can face high temperature, the temperature is often in the range of tens degree to several Baidu even thousands of degree.In order to cope with by
The variation of the performance of material caused by the variation of external environment, the buoyant material should have good temperature tolerance.It is asked based on above-mentioned
Topic, preparing has the research emphasis for becoming today's society compared with the solid buoyancy material of high temperature tolerance.
Summary of the invention
For the problem that solid buoyancy material temperature tolerance at this stage is poor, especially for can be used for deep-sea high temperature resistant solid
The demand of buoyant material, the present invention are prepared for a kind of floating bead/mullite solid buoyancy material with good heat-resisting quantity, the material
Material also has good heat-resisting quantity, the preparation method simple process of material, experiment in addition to having the characteristics that advantages of higher compressive strength
It is easy to operate, in experimentation the features such as contamination-free generation.
A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material, key step are as follows:
(1) pretreatment of floating bead:
Raw material is weighed, a certain amount of floating bead is put into distilled water, is stirred, after standing 5 ~ 10min, the floating bead on upper layer is taken
Out, it is placed in surface plate, is dried in 90 ~ 110 DEG C of electric drying oven with forced convection, it is spare；
(2) preparation of premixed liquid:
Using distilled water as solvent, acrylamide and N, N '-methylene-bisacrylamide are respectively monomer and crosslinking agent, according to certain
Proportion prepare premixed liquid；
(3) floating bead/mullite slurry preparation:
Phase transition of the matrix mullite from feed kaolin, a certain amount of kaolin is added in (2), through ball mill ball milling
After a certain period of time, it obtains that then floating bead being added in mixed liquor containing kaolinic mixed liquor, it is spare after mixing；
(4) floating bead/mullite buoyant material preparation:
A certain amount of ammonium persulfate is added in mixed slurry in (3), is stirred continuously, is then poured into slurry in mold simultaneously
Constantly oscillation, mold is placed in 40 ~ 50 DEG C of baking ovens, half-dried green body is obtained after demoulding to be formed, through certain temperature it is dry and
After sintering, floating bead/mullite solid buoyancy material has been obtained.
The particle diameter distribution of the floating bead is 80 ~ 200 mesh.
The solid concentration of the slurry is 0 ~ 50 wt.%.
The mass ratio of the kaolin and premixed liquid is 1:1 ~ 3:1.
Distilled water in the premixed liquid: acrylamide: proportion between N ' N methylene-bisacrylamide three be (80 ~
110) ml:(15~25) g:(1~3) g。
The citric acid of 1.5 ~ 2g is added in every 90 ~ 100ml slurry.
The concentration of the ammonium persulfate is 5 ~ 10 wt.%, and additional amount is that 1 ~ 3ml is added in every 100ml.
Described cube of six gang moulds tool is having a size of 20 ~ 30mm.
For the material from room temperature to 600 DEG C, heating rate is 0.5 ~ 2 DEG C/min, keeps the temperature 1 ~ 2h.
The sintering temperature of the material is 800 ~ 1300 DEG C, and soaking time is 1 ~ 3h.
A kind of high temperature resistant floating bead/mullite solid buoyancy material preparation method of the invention has the beneficial effect that
(1) this experiment can be played the role of reducing density to a certain extent using floating bead as filler material.
(2) citric acid being added in experiment, can play good peptizaiton to powder in slurry；
(3) using mullite as matrix in experiment, to prepare there is the buoyant material of heat-resisting quantity to provide guarantee.
(4) it is the floating bead of mullite as filler material using principal crystalline phase in experiment, raising material can be played to a certain extent
Durothermic effect.
(5) it can obtain having different mechanical performances, hot property and physics by adjusting the solid concentration in premixed liquid
The floating bead of performance/mullite solid buoyancy material.
(6) experimental method is simple, easy to operate, and the floating bead prepared using this method/mullite solid buoyancy material is had
There is higher temperature tolerance.
Detailed description of the invention
Fig. 1 is that floating bead/mullite solid buoyancy material that the solid concentration prepared in embodiment 1 is 50 wt.% passes through respectively
900 DEG C, 1000 DEG C and 1100 DEG C sintered scanning electron microscope diagrams.
Specific embodiment
Prepare premixed liquid using distilled water, acrylamide, N ' N methylene-bisacrylamide and citric acid as raw material, then to
A certain amount of kaolin is added in premix, a certain amount of floating bead is added after ball milling mixing is uniform, after being uniformly mixed
A certain amount of ammonium persulfate is added, is poured into mold, floating bead/not is obtained after the technical process such as molding, drying and sintering
Stone solid buoyancy material, present invention will be further explained below with reference to the attached drawings and examples.
Embodiment 1
A kind of floating bead/mullite solid buoyancy material preparation method, its step are as follows:
(1) preparation of premixed liquid
With distilled water, acrylamide in this embodiment, N ' N methylene-bisacrylamide and citric acid prepare premixed liquid, and three kinds
Ratio be 100ml:18g:1.8g:2g, it is spare；
(2) floating bead/mullite bodies preparation
A certain amount of kaolin is added into premixed liquid, after revolving speed is the planetary ball mill ball milling 4h of 600rpm, to mixing
A certain amount of floating bead is added in liquid, wherein the solid content in slurry is 50 wt.%, and the average grain diameter of floating bead is 80 μm, kaolinite
The quality of soil and premixed liquid is 2:1, the uniformly rear solution (0 ~ 1.5ml) that the ammonium persulfate that concentration is 10 wt.% is added to be mixed,
It stirs evenly, then by six gang mould of slurry cast to 20mm × 20mm × 20mm tool, through 40 DEG C of curing moldings, dries and be sintered
Afterwards, obtain that there is floating bead resistant to high temperature/mullite solid buoyancy material.
It is solid to be obtained into floating bead/mullite after being sintered under the conditions of 900 DEG C, 1000 DEG C and 1100 DEG C respectively for the green body of material
The density of body material is respectively 0.797,0.864 and 1.008g/cm3。
Claims (9)
1. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material, it is characterised in that: key step is as follows:
(1) pretreatment of floating bead:
Raw material is weighed, a certain amount of floating bead is put into distilled water, is stirred, after standing 5 ~ 10min, the floating bead on upper layer is taken
Out, it is placed in surface plate, is dried in 90 ~ 110 DEG C of electric drying oven with forced convection, it is spare；
(2) preparation of premixed liquid:
Using distilled water as solvent, acrylamide and N, N '-methylene-bisacrylamide are respectively monomer and crosslinking agent, according to certain
Proportion prepare premixed liquid；
(3) floating bead/mullite slurry preparation:
Phase transition of the matrix mullite from feed kaolin, a certain amount of kaolin is added in (2), through ball mill ball milling
After a certain period of time, it obtains that then floating bead being added in mixed liquor containing kaolinic mixed liquor, it is spare after mixing；
(4) floating bead/mullite solid buoyancy material preparation:
A certain amount of ammonium persulfate is added in mixed slurry in (3), is stirred continuously, is then poured into slurry in mold simultaneously
Constantly oscillation, mold is placed in 40 ~ 50 DEG C of baking ovens, half-dried green body is obtained after demoulding to be formed, through certain temperature it is dry and
After sintering, floating bead/mullite solid buoyancy material has been obtained.
2. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: the particle diameter distribution of fly ash float is 80 ~ 200 mesh.
3. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: the solid concentration of slurry is 0 ~ 50 wt.%.
4. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: the mass ratio of kaolin and premixed liquid is 1:1 ~ 3:1.
5. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: distilled water in premixed liquid: acrylamide: the proportion between N ' N methylene-bisacrylamide three is (80 ~ 110) ml:(15
~25) g:(1~3) g。
6. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: the citric acid of 1.5 ~ 2g is added in every 90 ~ 100ml slurry.
7. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: the concentration of ammonium persulfate is 5 ~ 10 wt.%, and additional amount is that 1 ~ 3ml is added in every 100ml.
8. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: cube six gang moulds tool is having a size of 20 ~ 30mm.
9. a kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material according to claim 1, feature exist
In: for material from room temperature to 600 DEG C, heating rate is 0.5 ~ 2 DEG C/min, keeps the temperature 1 ~ 2h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711004193.8A CN109694240A (en) | 2017-10-24 | 2017-10-24 | A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material |
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| CN201711004193.8A CN109694240A (en) | 2017-10-24 | 2017-10-24 | A kind of preparation method of high temperature resistant floating bead/mullite solid buoyancy material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349481A (en) * | 2021-11-29 | 2022-04-15 | 天津大学（青岛）海洋工程研究院有限公司 | Buoyancy material capable of resisting temperature of 1500 ℃ and preparation method thereof |
| CN114751739A (en) * | 2022-04-07 | 2022-07-15 | 陕西国防工业职业技术学院 | Process for preparing light building material by using fly ash |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106037A (en) * | 1985-08-13 | 1987-04-08 | 哈尔滨船舶工程学院 | Buoyancy material |
| CN101870588A (en) * | 2009-04-21 | 2010-10-27 | 河北勇龙邦大新材料有限公司 | Method and device for preparing hollow ceramic microspheres |
| CN102515820A (en) * | 2011-12-06 | 2012-06-27 | 天津大学 | Environment-friendly lightweight porous mullite ceramic and preparation method thereof |
| CN103951354A (en) * | 2014-05-15 | 2014-07-30 | 清华大学 | Cement-based buoyancy material and preparation method thereof |
| CN103979938A (en) * | 2014-04-25 | 2014-08-13 | 上海卫蓝海洋材料科技有限公司 | Deep-sea pressure resistant alumina ceramic hollow floating ball and preparation method thereof |
| CN104446203A (en) * | 2014-11-28 | 2015-03-25 | 天津中材工程研究中心有限公司 | Inorganic non-metallic solid buoyancy material and producing method thereof |
-
2017
- 2017-10-24 CN CN201711004193.8A patent/CN109694240A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85106037A (en) * | 1985-08-13 | 1987-04-08 | 哈尔滨船舶工程学院 | Buoyancy material |
| CN101870588A (en) * | 2009-04-21 | 2010-10-27 | 河北勇龙邦大新材料有限公司 | Method and device for preparing hollow ceramic microspheres |
| CN102515820A (en) * | 2011-12-06 | 2012-06-27 | 天津大学 | Environment-friendly lightweight porous mullite ceramic and preparation method thereof |
| CN103979938A (en) * | 2014-04-25 | 2014-08-13 | 上海卫蓝海洋材料科技有限公司 | Deep-sea pressure resistant alumina ceramic hollow floating ball and preparation method thereof |
| CN103951354A (en) * | 2014-05-15 | 2014-07-30 | 清华大学 | Cement-based buoyancy material and preparation method thereof |
| CN104446203A (en) * | 2014-11-28 | 2015-03-25 | 天津中材工程研究中心有限公司 | Inorganic non-metallic solid buoyancy material and producing method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 黄春舒等: "莫来石基轻质、气密型隔热陶瓷制备", 《稀有金属材料与工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114349481A (en) * | 2021-11-29 | 2022-04-15 | 天津大学（青岛）海洋工程研究院有限公司 | Buoyancy material capable of resisting temperature of 1500 ℃ and preparation method thereof |
| CN114751739A (en) * | 2022-04-07 | 2022-07-15 | 陕西国防工业职业技术学院 | Process for preparing light building material by using fly ash |
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