CN114671669A - Alumina hydrogel and preparation method thereof, and transparent adjustable intelligent ceramic - Google Patents
Alumina hydrogel and preparation method thereof, and transparent adjustable intelligent ceramic Download PDFInfo
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- 239000000017 hydrogel Substances 0.000 title claims abstract description 74
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 title claims abstract description 11
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910052796 boron Inorganic materials 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 22
- -1 hydroxyl aluminum hydrate Chemical compound 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims description 56
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- FGUJWQZQKHUJMW-UHFFFAOYSA-N [AlH3].[B] Chemical compound [AlH3].[B] FGUJWQZQKHUJMW-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000004327 boric acid Substances 0.000 claims description 8
- HXITXNWTGFUOAU-UHFFFAOYSA-N phenylboronic acid Chemical compound OB(O)C1=CC=CC=C1 HXITXNWTGFUOAU-UHFFFAOYSA-N 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 6
- VGTPKLINSHNZRD-UHFFFAOYSA-N oxoborinic acid Chemical compound OB=O VGTPKLINSHNZRD-UHFFFAOYSA-N 0.000 claims description 5
- YDMRDHQUQIVWBE-UHFFFAOYSA-N (2-hydroxyphenyl)boronic acid Chemical compound OB(O)C1=CC=CC=C1O YDMRDHQUQIVWBE-UHFFFAOYSA-N 0.000 claims description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- OBQRODBYVNIZJU-UHFFFAOYSA-N (4-acetylphenyl)boronic acid Chemical compound CC(=O)C1=CC=C(B(O)O)C=C1 OBQRODBYVNIZJU-UHFFFAOYSA-N 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 230000002441 reversible effect Effects 0.000 description 25
- 230000007704 transition Effects 0.000 description 15
- 239000000499 gel Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 229940024545 aluminum hydroxide Drugs 0.000 description 10
- 230000008569 process Effects 0.000 description 9
- 230000008859 change Effects 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000013329 compounding Methods 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000001338 self-assembly Methods 0.000 description 3
- 239000003086 colorant Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 230000004043 responsiveness Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 210000002808 connective tissue Anatomy 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- WMWXXXSCZVGQAR-UHFFFAOYSA-N dialuminum;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3] WMWXXXSCZVGQAR-UHFFFAOYSA-N 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 210000004872 soft tissue Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012800 visualization Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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Classifications
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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
- C04B35/10—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 aluminium oxide
-
- 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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/624—Sol-gel processing
-
- 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
- C04B2235/02—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
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
-
- 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
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
Abstract
The disclosure provides an alumina hydrogel and a preparation method thereof, and a transparent adjustable intelligent ceramic prepared from the alumina hydrogel. A method for preparing alumina hydrogel comprises adding boron-containing compound into solvent to obtain boron-containing solution, wherein the concentration of boron in the boron-containing solution is greater than critical concentration; and adding a hydroxyl aluminum hydrate to the boron-containing solution to obtain a final solution, wherein the concentration of boron is greater than the critical concentration and the boron is uniformly dispersed.
Description
Technical Field
The disclosure relates to an alumina hydrogel and a preparation method thereof, and a transparent adjustable intelligent ceramic prepared from the alumina hydrogel.
Background
Hydrogels are a class of very hydrophilic three-dimensional network-structured gels that swell rapidly in water and in this swollen state can hold a large volume of water without dissolving. The aluminum oxide has the characteristics of high hardness, good wear resistance, stable physical and chemical properties, strong corrosion resistance, long-term stable existence in a body fluid environment, excellent biological inertia, biocompatibility and the like. Hydrogels are widely used clinically as soft tissue replacements, particularly soft connective tissue materials. In addition, the hydrogel with transparency adjustability has a good development prospect in the field of transparent visualization.
Disclosure of Invention
The disclosure provides an alumina hydrogel and a preparation method thereof, and a transparent adjustable intelligent ceramic prepared from the alumina hydrogel.
According to a first aspect of the present disclosure, a method of preparing an alumina hydrogel comprises adding a boron-containing compound to a solvent to obtain a boron-containing solution, wherein the concentration of boron in the boron-containing solution is greater than a critical concentration; and adding a hydroxyl aluminum hydrate into the boron-containing solution to obtain a final solution, wherein the concentration of boron in the final solution is greater than the critical concentration and the final solution is uniformly dispersed.
According to at least one embodiment of the present disclosure, the concentration of the aluminum hydroxide hydrate in the final solution is 10 to 500 mg/ml.
According to at least one embodiment of the present disclosure, the final solution is prepared at 15 to 35 ℃.
According to at least one embodiment of the present disclosure, the boron-containing compound is at least one of borax, boric acid, metaboric acid, phenylboronic acid, p-acetylphenylboronic acid, hydroxyphenylboronic acid.
According to at least one embodiment of the present disclosure, the solvent is at least one of water, methanol, ethanol, isopropanol, tert-butanol.
According to at least one embodiment of the present disclosure, the boron to aluminum ratio in the final solution is between 1:2 and 1: 10.
According to at least one embodiment of the present disclosure, the method of making further comprises adding a third non-transparent component to the boron-containing solution prior to adding the aluminum hydroxide hydrate, resulting in a mixed solution.
According to at least one embodiment of the present disclosure, the third non-transparent is at least one of silica, zirconia, yttria.
According to a second aspect of the disclosure, the alumina hydrogel is prepared according to the preparation method, and the boron-aluminum ratio of the alumina hydrogel is 1: 2-1: 10.
According to a third aspect of the present disclosure, a transparent tunable smart ceramic is prepared from the above alumina hydrogel.
Drawings
The accompanying drawings, which are included to provide a further understanding of the disclosure and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the disclosure and together with the description serve to explain the principles of the disclosure.
Fig. 1 is a flow diagram of alumina hydrogel preparation according to at least one embodiment of the present disclosure.
FIG. 2 is a graph of boron to aluminum ratio in alumina hydrogel versus sol-gel phase transition temperature in accordance with at least one embodiment of the present disclosure.
Detailed Description
The present disclosure will be described in further detail with reference to the drawings and embodiments. It is to be understood that the specific embodiments described herein are for purposes of illustration only and are not to be construed as limitations of the present disclosure. It should be further noted that, for the convenience of description, only the portions relevant to the present disclosure are shown in the drawings.
It should be noted that the embodiments and features of the embodiments in the present disclosure may be combined with each other without conflict. The present disclosure will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
The invention provides a temperature-sensitive aluminum oxide reversible hydrogel and a preparation method and application thereof. A three-dimensional network type multi-element gel composite system is obtained by mixing boric acid, metaboric acid, boron-containing organic matters and other boron-containing compounds, a solvent and an aluminum hydroxide water polymer, and a material with reversible sol-gel conversion performance along with the change of temperature is successfully prepared by utilizing the temperature responsiveness of a boric acid ester bond and combining the multi-active functional groups of the aluminum hydroxide water polymer, and can be used as a thermal management gel to realize the release and control of heat.
In at least one embodiment of the present disclosure, the present disclosure provides a method of preparing an alumina hydrogel, as shown in fig. 1, comprising
S1: adding a boron-containing compound into a solvent to obtain a boron-containing solution, wherein the concentration of boron in the boron-containing solution is greater than the self-assembly critical concentration of the boron-containing solution.
S2: and adding a hydroxyl aluminum hydrate into the boron-containing solution to obtain a final solution, wherein the concentration of boron in the final solution is greater than the self-assembly critical concentration of the boron and the boron is uniformly dispersed, and the final solution is the alumina hydrogel.
Wherein the second step S2 is referred to as compounding. The compounding condition is to ensure that the boron concentration in the alumina hydrogel (final solution) is greater than the self-assembly critical concentration and the alumina hydrogel is uniformly dispersed.
The boron-containing compound in the boron-containing solution may associate from individual ions or molecules into colloidal aggregates, i.e. gels, when it exceeds a certain concentration. The concentration at which a sudden change in the properties of the solution occurs, i.e. the concentration of the solution at which gel formation begins, is called the critical concentration.
To ensure a homogeneous gel, the solution was stirred well after each mixing and allowed to stand for a sufficient period of time.
The aluminum hydroxide hydrate can also be dissolved in an active solvent firstly, fully homogenized and stirred to obtain an aluminum hydroxide active solution, and then mixed with the boron-containing solution according to the compounding conditions.
The concentration of the aluminum hydroxide hydrate in the final solution is 10-500 mg/ml.
The final state solution is subjected to sexual compounding at the temperature of 15-35 ℃ to obtain the alumina hydrogel.
The boron-containing compound can be at least one of borax, boric acid, metaboric acid, phenylboronic acid, p-acetylphenylboronic acid and hydroxyphenylboronic acid.
The solvent is at least one of water, methanol, ethanol, isopropanol and tert-butanol. For example, deionized water, absolute ethanol, or a 1:1 mixture of deionized water and ethanol may be selected as the solvent.
According to another embodiment of the present disclosure, the boron to aluminum ratio in the alumina hydrogel is between 1:2 and 1: 10. The preparation of the reversible hydrogel is realized between the boron-containing solution and the aluminum hydroxide hydrogel through multiple hydrogen bonds. The proportion of boron and aluminum in the hydrogel is adjusted to obtain hydrogels with different phase transition temperatures, namely, the difference of boron and aluminum ratios can affect the sol-gel phase transition temperature of the alumina hydrogel, and the relationship is shown in fig. 2. When the boron-aluminum ratio is increased, the phase transition temperature is increased. Therefore, alumina hydrogels with different phase transition temperatures can be prepared by adjusting the boron-aluminum ratio in the gel.
For example, when the boron-aluminum ratio is 1:10 and the temperature of the final solution is less than or equal to 36 ℃, obtaining hydrogel; when the temperature of the final state solution is more than 36 ℃, the sol is obtained. When the final solution is cooled to below 36 ℃, the solution loses fluidity and hydrogel can be formed; when the temperature is more than 36 ℃, the fluidity is recovered. And under the concentration, the single boron-containing solution or the single aluminum hydroxide aqueous polymer solution still has good fluidity after being heated, and can not form hydrogel.
According to yet another embodiment of the present disclosure, the method of preparing further comprises adding a third non-transparent component to the boron-containing solution prior to adding the aluminum oxide hydrate (S2) to obtain a mixed solution. Then, to this mixed solution, a hydroxyaluminum hydrate was added to obtain a final state solution, i.e., an alumina hydrogel. The third non-transparent component includes, but is not limited to, silicon oxide, zirconium oxide, yttrium oxide, etc., and one or more combinations may be added. The examples show that by adding 10% to 50% silica content to the boron containing solution, the transparency of the final alumina hydrogel will be reduced by 10% to 60%. That is, the amount of the third non-transparent component added can be adjusted to obtain reversible hydrogels of varying transparency. Meanwhile, the addition of the third non-transparent component also influences the phase transition temperature of the hydrogel (which can be changed between 36 and 80 ℃).
The selection range of the third component is wide, a great deal of selectivity is provided, and the preparation of intelligent ceramics with different colors, transparencies, brightness and the like can be conveniently realized.
According to a second aspect of the present disclosure, an alumina hydrogel is provided, which is prepared according to the above preparation method, has a boron-aluminum ratio of 1:2 to 1:10, and is a temperature-responsive reversible hydrogel (thermosensitive hydrogel). That is, the hydrogel may achieve a reversible transition between hydrogel and sol with temperature change.
According to a third aspect of the disclosure, a transparent tunable smart ceramic is provided, which is prepared from the above alumina hydrogel, and can obtain smart ceramics with different phase transition temperatures by adjusting the boron-aluminum ratio in the hydrogel, and can also obtain smart ceramics with different colors, transparencies and brightnesses by adding third non-transparent components of different types and concentrations.
The temperature response type reversible hydrogel can also be applied to the energy storage direction, the final-state solution is gelatinized, the sol is formed again after heat absorption through the phase change point, energy is absorbed and stored in the phase change process, and when the sol is placed in a cold environment (the temperature is lower than the phase change point), the sol releases heat and forms gel again.
The technical solution of the present disclosure is further described in detail by several embodiments in conjunction with the accompanying drawings. However, the selected examples are merely illustrative of the present disclosure and do not limit the scope of the present disclosure.
Example 1
The embodiment prepares the temperature-sensitive reversible alumina hydrogel, and the specific process is as follows:
(1) 0.5g of boric acid is added into deionized water, and after uniform stirring, a boron-containing aqueous solution is obtained.
(2) And (2) adding a hydroxyl aluminum hydrate with the boron-aluminum ratio of 1:10 into the boron-containing aqueous solution obtained in the step (1), fully stirring at 20 ℃, and standing to obtain the temperature-sensitive reversible hydrogel. The result of testing the temperature-sensitive characteristic of the temperature-sensitive reversible hydrogel obtained in the step (2) is shown in fig. 2.
Example 2
The embodiment prepares the temperature-sensitive reversible alumina hydrogel, and the specific process is as follows:
(1) 0.5g of metaboric acid is added into deionized water and stirred evenly to obtain the aqueous solution containing boron.
(2) Adding a hydroxyl aluminum hydrate with the boron-aluminum ratio of 1:5 into the boron-containing aqueous solution obtained in the step (1), fully stirring at 20 ℃, and standing to obtain the temperature-sensitive reversible hydrogel.
The experimental results are comparable to example 1.
Example 3
The embodiment prepares the temperature-sensitive reversible alumina hydrogel, and the specific process comprises the following steps:
(1) adding 1g of p-phenylboronic acid into absolute ethyl alcohol, and uniformly stirring to obtain a boron-containing alcohol solution.
(2) Adding a hydroxyl aluminum hydrate with the boron-aluminum ratio of 1:5 into the boron-containing alcoholic solution obtained in the step (1), fully stirring at 35 ℃, and standing to obtain the temperature-sensitive reversible hydrogel.
The experimental result is equivalent to that of example 1, and the phase transition temperature is 53 DEG C
Example 4
The embodiment prepares the temperature-sensitive reversible alumina hydrogel, and the specific process comprises the following steps:
(1) adding 2g of hydroxyphenylboronic acid into a mixed solvent of ethanol and water in a ratio of 1:1, and uniformly stirring to obtain a boron-containing mixed solution.
(2) Adding a hydroxyl aluminum hydrate with the boron-aluminum ratio of 1:7 into the boron-containing aqueous solution obtained in the step (1), fully stirring at 30 ℃, and standing to obtain the temperature-sensitive reversible hydrogel.
The experimental result is equivalent to that of example 1, and the phase transition temperature is 46 DEG C
Example 5
The embodiment prepares the temperature-sensitive reversible alumina hydrogel, and the specific process is as follows:
(1) adding 1g of boric acid into deionized water, and stirring uniformly to obtain a boron-containing solution.
(2) And (2) adding 50% of gas-phase silicon oxide into the boron-containing solution obtained in the step (1) to obtain a mixed solution.
(3) Adding a hydroxyl aluminum hydrate with the boron-aluminum ratio of 1:10 into the mixed solution obtained in the step (2), fully stirring at 20 ℃, and standing to obtain the temperature-sensitive reversible hydrogel.
The results are comparable to example 1, with a phase transition temperature of 44 ℃ and a 35% reduction in transparency.
Example 6
The embodiment prepares the temperature-sensitive reversible alumina hydrogel, and the specific process comprises the following steps:
(1) and adding 2g of boric acid into deionized water, and uniformly stirring to obtain a boron-containing solution.
(2) And (2) adding 10% of gas-phase silicon oxide into the boron-containing solution obtained in the step (1) to obtain a mixed solution.
(3) Adding a hydroxyl aluminum hydrate with the boron-aluminum ratio of 1:4 into the mixed solution obtained in the step (2), fully stirring at 20 ℃, and standing to obtain the temperature-sensitive reversible hydrogel.
The results of the experiment are comparable to example 5, with a phase transition temperature of 62 ℃ and a 10% reduction in transparency.
Example 7
The embodiment prepares the temperature-sensitive reversible alumina hydrogel, and the specific process is as follows:
(1) 0.5g of phenylboronic acid is added into absolute ethyl alcohol and stirred uniformly to obtain a boron-containing solution.
(2) Adding 20% of gas-phase silicon oxide into the boron-containing solution obtained in the step (1) to obtain a mixed solution
(3) Adding a hydroxyl aluminum hydrate with the boron-aluminum ratio of 1:8 into the mixed solution obtained in the step (2), fully stirring at 30 ℃, and standing to obtain the temperature-sensitive reversible hydrogel.
The results are comparable to example 5, with a phase transition temperature of 42 ℃ and a 25% reduction in transparency.
The positive and beneficial effects of the present disclosure are: (1) the method realizes the preparation of the reversible hydrogel with temperature responsiveness by a physical crosslinking method between the boron-containing compound and the aluminum hydroxide hydrate, and is simple and easy to implement; (2) the preparation method disclosed by the invention has the advantages that the types of the boron-containing compounds which can be selected are various, and the sources are wide; (3) the phase transition temperature of the temperature response type reversible hydrogel is adjustable and controllable, and the sol-gel transition process of the hydrogel can be realized through the change of the external temperature, so that the temperature response type reversible hydrogel can be used in the field of intelligent hydrogel transparent display.
It will be understood by those skilled in the art that the foregoing embodiments are merely for clarity of illustration of the disclosure and are not intended to limit the scope of the disclosure. Other variations or modifications may occur to those skilled in the art, based on the foregoing disclosure, and are still within the scope of the present disclosure.
Claims (10)
1. The preparation method of the alumina hydrogel is characterized by comprising the steps of adding a boron-containing compound into a solvent to obtain a boron-containing solution, wherein the concentration of boron in the boron-containing solution is greater than a critical concentration; and
and adding a hydroxyl aluminum hydrate into the boron-containing solution to obtain a final solution, wherein the concentration of boron in the final solution is greater than the critical concentration and the final solution is uniformly dispersed.
2. The method of claim 1, wherein the concentration of aluminum hydroxide hydrogel in the final solution is 10 to 500 mg/ml.
3. The method for preparing the alumina hydrogel according to claim 1, wherein the final solution is prepared at 15 to 35 ℃.
4. The method of claim 1, wherein the boron-containing compound is at least one of borax, boric acid, metaboric acid, phenylboronic acid, terephthaloboric acid, p-acetylphenylboronic acid, and hydroxyphenylboronic acid.
5. The method of claim 1, wherein the solvent is at least one of water, methanol, ethanol, isopropanol, and tert-butanol.
6. The method for preparing the alumina hydrogel according to claim 1, wherein the boron-aluminum ratio in the final solution is 1:2 to 1: 10.
7. The method of claim 1 further comprising adding a third non-transparent component to the boron-containing solution prior to adding the aluminum hydroxide hydrogel to provide a mixed solution.
8. The method of claim 7, wherein the third non-transparent component is at least one of silica, zirconia, yttria.
9. An alumina hydrogel prepared by the preparation method of any one of claims 1 to 8, wherein the boron-aluminum ratio of the alumina hydrogel is 1: 2-1: 10.
10. A transparent tunable smart ceramic prepared from the alumina hydrogel of claim 9.
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| CN (1) | CN114671669A (en) |
Citations (7)
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| US5122565A (en) * | 1990-10-26 | 1992-06-16 | Shell Oil Company | Stabilized polyketone polymers containing a mixture of a hydroxyapatite and an alumina hydrogel |
| US5804213A (en) * | 1991-10-09 | 1998-09-08 | Lectec Corporation | Biologically active aqueous gel wound dressing |
| WO2006112533A1 (en) * | 2005-04-18 | 2006-10-26 | Showa Denko K.K. | Water-containing gel form and production method thereof |
| JP2008074925A (en) * | 2006-09-20 | 2008-04-03 | Kawamura Inst Of Chem Res | Borate group-containing organic inorganic composite hydrogel and method for producing the same |
| CN104311859A (en) * | 2014-10-10 | 2015-01-28 | 齐鲁工业大学 | Preparation method of high-strength dual-mesh nano-meter aluminum oxide composite hydrogel |
| CN109517309A (en) * | 2018-11-09 | 2019-03-26 | 福建农林大学 | A kind of preparation method of plant polyphenol nano-cellulose antibacterial self-healing hydrogel |
| CN112940294A (en) * | 2021-03-18 | 2021-06-11 | 中北大学 | PVA/HA double-network hydrogel and preparation method and application thereof |
-
2022
- 2022-03-02 CN CN202210198925.6A patent/CN114671669A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5122565A (en) * | 1990-10-26 | 1992-06-16 | Shell Oil Company | Stabilized polyketone polymers containing a mixture of a hydroxyapatite and an alumina hydrogel |
| US5804213A (en) * | 1991-10-09 | 1998-09-08 | Lectec Corporation | Biologically active aqueous gel wound dressing |
| WO2006112533A1 (en) * | 2005-04-18 | 2006-10-26 | Showa Denko K.K. | Water-containing gel form and production method thereof |
| JP2008074925A (en) * | 2006-09-20 | 2008-04-03 | Kawamura Inst Of Chem Res | Borate group-containing organic inorganic composite hydrogel and method for producing the same |
| CN104311859A (en) * | 2014-10-10 | 2015-01-28 | 齐鲁工业大学 | Preparation method of high-strength dual-mesh nano-meter aluminum oxide composite hydrogel |
| CN109517309A (en) * | 2018-11-09 | 2019-03-26 | 福建农林大学 | A kind of preparation method of plant polyphenol nano-cellulose antibacterial self-healing hydrogel |
| CN112940294A (en) * | 2021-03-18 | 2021-06-11 | 中北大学 | PVA/HA double-network hydrogel and preparation method and application thereof |
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Application publication date: 20220628 |