CN116354710A - Method for preparing ceramic by pouring poly-gamma-glutamic acid gel - Google Patents
Method for preparing ceramic by pouring poly-gamma-glutamic acid gel Download PDFInfo
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- CN116354710A CN116354710A CN202310143432.7A CN202310143432A CN116354710A CN 116354710 A CN116354710 A CN 116354710A CN 202310143432 A CN202310143432 A CN 202310143432A CN 116354710 A CN116354710 A CN 116354710A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 72
- 239000004220 glutamic acid Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 21
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 28
- 238000005266 casting Methods 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 13
- 238000011065 in-situ storage Methods 0.000 claims abstract description 11
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 10
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 9
- 239000011268 mixed slurry Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052661 anorthite Inorganic materials 0.000 claims abstract description 3
- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 claims abstract description 3
- 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 3
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 3
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 3
- 238000010382 chemical cross-linking Methods 0.000 claims description 9
- 230000002255 enzymatic effect Effects 0.000 claims description 6
- 238000004132 cross linking Methods 0.000 claims description 5
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 5
- CUGZWHZWSVUSBE-UHFFFAOYSA-N 2-(oxiran-2-ylmethoxy)ethanol Chemical compound OCCOCC1CO1 CUGZWHZWSVUSBE-UHFFFAOYSA-N 0.000 claims description 3
- 108010001336 Horseradish Peroxidase Proteins 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 239000004088 foaming agent Substances 0.000 claims description 3
- FPQQSJJWHUJYPU-UHFFFAOYSA-N 3-(dimethylamino)propyliminomethylidene-ethylazanium;chloride Chemical compound Cl.CCN=C=NCCCN(C)C FPQQSJJWHUJYPU-UHFFFAOYSA-N 0.000 claims description 2
- 229920001661 Chitosan Polymers 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 102000009097 Phosphorylases Human genes 0.000 claims description 2
- 108010073135 Phosphorylases Proteins 0.000 claims description 2
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 239000007787 solid Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 239000000178 monomer Substances 0.000 description 5
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 4
- 229910021426 porous silicon Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 1
- 229920001817 Agar Polymers 0.000 description 1
- 206010029350 Neurotoxicity Diseases 0.000 description 1
- 206010044221 Toxic encephalopathy Diseases 0.000 description 1
- 239000008272 agar Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010410 dusting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004421 molding of ceramic Methods 0.000 description 1
- 230000007135 neurotoxicity Effects 0.000 description 1
- 231100000228 neurotoxicity Toxicity 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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Abstract
The invention relates to a method for preparing ceramic by gel casting of poly-gamma-glutamic acid, belonging to the technical field of ceramic preparation. Dissolving poly-gamma-glutamic acid in water, then adding ceramic powder, fully mixing, adjusting the pH value of mixed slurry to 2-7, adding a cross-linking agent, fully stirring, injecting the obtained slurry into a grinding tool, carrying out in-situ polymerization to obtain a ceramic green body with a macromolecular network structure, and sintering to obtain ceramic; the ceramic powder is one or more of mullite, silicon nitride, silicon carbide, zirconium boride, aluminum oxide and anorthite. The invention is used as a gel casting system with green environmental protection, high solid load and low viscosity, and is used for preparing ceramic elements with high quality and complex shape. The poly-gamma-glutamic acid gel system has a unique three-dimensional network structure, can realize the preparation of high-performance and high-precision ceramics, and is convenient for popularization and application.
Description
Technical Field
The invention belongs to the technical field of ceramic preparation, and particularly relates to a method for preparing ceramic by gel casting of poly-gamma-glutamic acid.
Background
The colloid forming technology can improve the uniformity of the ceramic body and reduce the defect of bad microstructure, is suitable for manufacturing ceramic elements with complex shapes, and has important position in the ceramic process. Among them, gel casting belongs to one of the colloid processing, has a great advantage, and has been applied to the preparation of dense and porous ceramic elements at present. The gel casting combines the traditional molding of ceramic slurry with polymer chemistry, forms a macromolecular network through in-situ polymerization, and solidifies ceramic particles together to obtain a ceramic element with high quality and complex shape, which is a low-consumption, pressureless and near-net molding technology and can replace the traditional casting molding technology. The choice of polymer is critical in the overall casting process in order to meet the requirements of high solids content, low viscosity of the ceramic suspension.
The earliest water-soluble monomers used for gel casting include acrylamide and methacrylamide, which can obtain green bodies with high mechanical strength, but the main problem of using acrylamide monomers is neurotoxicity, which causes irreversible damage to human body and environment. Other gelling systems, including 2-hydroxyethyl acrylate, N-dimethylacrylamide, etc., also exhibit some toxicity and cause an increase in the number of organic phases in the ceramic suspension, while being insufficiently resistant to oxygen inhibition, resulting in green scaling, dusting, etc. For these reasons, many researchers have attempted to overcome these limitations and replace toxic monomers with other gelling systems, such as: polysaccharides, agar, proteins, these systems still exhibit disadvantages such as low solids loading in the slurry, long gelation time and relatively large temperature influence, thus limiting their widespread use.
Disclosure of Invention
In order to effectively solve the problems of more toxic monomers, more organic reagents, low solid load, long gelation time and larger influence by temperature in the traditional gel casting system and realize the preparation of the ceramic with high cost performance by using the gel casting method, the invention aims at preparing the ceramic with high cost performance by using the green efficient gel casting method, provides a gel system which takes the synthesized poly-gamma-glutamic acid produced by microbial fermentation in a large scale as the gel monomer, realizes the preparation method with high solid load, low viscosity and environmental protection, and is applied to the preparation of ceramic products with various performances.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the method for preparing ceramic by pouring poly-gamma-glutamic acid gel comprises the steps of dissolving poly-gamma-glutamic acid in water, adding ceramic powder, fully mixing, adjusting the pH value of mixed slurry to 2-7, adding a cross-linking agent, fully stirring, injecting the obtained slurry into a grinding tool, performing in-situ polymerization to obtain a ceramic green body with a macromolecular network structure, and sintering to obtain ceramic;
the ceramic powder is one or more of mullite, silicon nitride, silicon carbide, zirconium boride, aluminum oxide and anorthite.
Further, the mass ratio of the poly-gamma-glutamic acid to the ceramic powder to the cross-linking agent to the water is 4-6:60-65:1-3:26-35.
Further, the pH value of the mixed slurry is regulated by dripping 1M dilute hydrochloric acid.
Further, the cross-linking agent is one of a physical cross-linking agent, a chemical cross-linking agent and an enzymatic cross-linking agent.
Further, the physical cross-linking agent is one of glycidyl methacrylate, adipic acid dihydrazide and chitosan.
Further, the condition for in-situ polymerization after adding the physical crosslinking agent is ultraviolet radiation, and 365 nm ultraviolet light is used for irradiating 2 h.
Further, the chemical cross-linking agent is one of ethylene glycol glycidyl ether, glycidyl methacrylate and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride.
Further, the foaming agent sodium dodecyl sulfate is added simultaneously after the chemical cross-linking agent is added, and the dosage is 0.1 wt percent of the ceramic powder.
Further, the chemical cross-linking agent is added to react at the temperature of 20-60 ℃ for 1-2 h when in-situ polymerization occurs.
Further, the enzymatic cross-linking agent is one of horseradish peroxidase and phosphorylase.
Further, the time required for the enzymatic crosslinking at 40℃was 5.+ -. 2s.
Further, the sintering conditions are: the sintering temperature is 1500-1600 ℃ and the sintering time is 1-3 h.
Further, the ceramics prepared by the preparation method can be used as heat insulation ceramics, wave-absorbing ceramics, biological ceramics, high-temperature ceramics, transparent ceramics and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. the physical crosslinking method is formed by the static action, the hydrogen bonding action and the specific bonding action between molecules under 365 and nm ultraviolet irradiation without adding excessive reagents such as an initiator, a catalyst and the like into a system, and the gel blank can be obtained by simply mixing the precursor solution and the ceramic powder, so that the gel blank has stronger chemical selectivity.
2. In addition, the enzyme-participated crosslinking is to form gel rapidly through in-situ reaction with grafted poly-gamma-glutamic acid, so that the condition is milder, the gel can be gelled rapidly within a few seconds, and the gel has high efficiency and specificity.
3. The invention can realize the preparation of high-performance and high-precision ceramics and is convenient for popularization and application.
Drawings
FIG. 1 is a sample of alumina prepared from an acrylamide gel system;
fig. 2 is a green body prepared in example 2 of the present invention.
Description of the embodiments
The technical solution and effects of the present invention will be further described with reference to the accompanying drawings and specific embodiments, but the scope of the present invention is not limited thereto.
Examples
The preparation method of the porous silicon nitride ceramic of the embodiment comprises the following steps: dissolving 6 g poly-gamma-glutamic acid in 28 mL water, adding 65g of silicon nitride ceramic powder, fully mixing, adjusting the pH value of the mixed slurry to 2, adopting a chemical crosslinking method, adding 1g of ethylene glycol glycidyl ether as a crosslinking agent, adding 0.065g of sodium dodecyl sulfate serving as a foaming agent, fully stirring to obtain 0.5 Pa.S low-viscosity slurry, injecting the slurry into a grinding tool, reacting for 20 min at 50 ℃, and carrying out in-situ polymerization to obtain the porous silicon nitride ceramic green body. Because of the relatively low viscosity, the slurry fills the whole die, the compressive strength of the green body is 20MPa, the flexural strength is as high as 13 MPa, the surface is free from powder falling and peeling. The porous silicon nitride ceramic with the porosity of 76.5% is obtained by sintering for 2 hours at 1600 ℃, the sintering shrinkage rate is only 0.5%, the heat conductivity coefficient is as low as 0.168W/m.k, and the porous silicon nitride ceramic has good application prospect as heat insulation ceramic.
Examples
The preparation method of the alumina ceramic of the embodiment comprises the following steps: dissolving 4 g poly-gamma-glutamic acid in 33 mL water, adding 60g of alumina ceramic powder, fully mixing, adjusting the pH of the mixed slurry to 5, adopting an enzymatic method to crosslink, adding 3g of horseradish peroxidase as a crosslinking agent, fully stirring the low-viscosity slurry of 0.34 Pa.S, injecting the low-viscosity slurry into a mould, placing the mould in a constant temperature oven at 40 ℃ for reacting for 7S, and carrying out in-situ polymerization to obtain an alumina ceramic green body, wherein the compressive strength of the green body is 42.14 MPa, the surface of the green body has no powder dropping and no peeling phenomenon, and the green body is shown in figure 2. Sintering for 3 hours at 1600 ℃ to obtain the alumina ceramic with the compressive strength of 152 MPa, wherein the porosity is 8.64 percent, the sintering shrinkage rate is only 0.88 percent, and the alumina ceramic is successfully applied to the metallurgical field as high-temperature ceramic.
Examples
The preparation method of the silicon nitride ceramic of the embodiment comprises the following steps: 5g of poly-gamma-glutamic acid is dissolved in 29 mL water, then 65g of silicon nitride ceramic powder is added and fully mixed, the pH value of the mixed slurry is regulated to be 4, a physical crosslinking method is adopted, 1g of glycidyl methacrylate is added as a crosslinking agent and fully stirred to be 0.68 Pa.S of low-viscosity slurry, after the low-viscosity slurry is injected into a mould, the low-viscosity slurry is subjected to in-situ polymerization by 365 nm ultraviolet light irradiation 2h to obtain a silicon nitride ceramic green body, the compressive strength of the green body is 33.87 MPa, the flexural strength is up to 15.76 MPa, the surface of the green body is free from powder dropping and peeling phenomenon is avoided. The silicon nitride ceramic is obtained by sintering for 2 hours in nitrogen atmosphere at 1600 ℃, the compressive strength is up to 75 MPa, the flexural strength is 37.51 MPa, the sintering shrinkage is 1.32%, and the silicon nitride ceramic has good application prospect as a wave-absorbing ceramic.
Comparative example
This comparative example is different from example 2 in that the comparative example is an alumina sample prepared by an acrylamide gel system, and as shown in FIG. 1, the green body is obtained by standing for 24 hours at room temperature, and the green body has a flexural strength of 7.5MPa, a compressive strength of 12.8 MPa and serious surface peeling.
The foregoing is merely illustrative of specific embodiments of this invention, and the scope of the invention is not limited thereto, as modifications and substitutions will be readily made by those skilled in the art without departing from the principles of the invention, and are intended to be included within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A method for preparing ceramic by pouring poly-gamma-glutamic acid gel is characterized in that the method comprises the steps of dissolving poly-gamma-glutamic acid in water, then adding ceramic powder, fully mixing, adjusting the pH value of mixed slurry to 2-7, adding a cross-linking agent, fully stirring, injecting the obtained slurry into a grinding tool, carrying out in-situ polymerization to obtain a ceramic green body with a macromolecular network structure, and sintering to obtain ceramic;
the ceramic powder is one or more of mullite, silicon nitride, silicon carbide, zirconium boride, aluminum oxide and anorthite.
2. The method for preparing ceramic by casting poly-gamma-glutamic acid gel according to claim 1, wherein the mass ratio of poly-gamma-glutamic acid to ceramic powder to cross-linking agent to water is 4-6:60-65:1-3:26-35.
3. The method for preparing ceramic by gel casting of poly-gamma-glutamic acid according to claim 1, wherein the pH value of the mixed slurry is adjusted by dropping 1M diluted hydrochloric acid.
4. The method for preparing ceramic by casting poly-gamma-glutamic acid gel according to claim 1, wherein the cross-linking agent is one of a physical cross-linking agent, a chemical cross-linking agent and an enzymatic cross-linking agent.
5. The method for preparing ceramic by casting poly-gamma-glutamic acid gel according to claim 4, wherein the physical cross-linking agent is one of glycidyl methacrylate, adipic acid dihydrazide and chitosan, and the condition that in-situ polymerization occurs after the physical cross-linking agent is added is ultraviolet radiation, and 365 nm ultraviolet light is adopted to irradiate 2 h.
6. The method for preparing ceramic by casting poly-gamma-glutamic acid gel according to claim 4, wherein the chemical cross-linking agent is one of ethylene glycol glycidyl ether, glycidyl methacrylate and 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, and sodium dodecyl sulfate serving as a foaming agent is added at the same time after the chemical cross-linking agent is added, and the amount is 0.1 wt percent of ceramic powder.
7. The method for preparing ceramic by casting poly-gamma-glutamic acid gel according to claim 4, wherein the chemical cross-linking agent is added to react at a temperature of 20-60 ℃ for 1-2 h.
8. The method for preparing ceramic by casting poly-gamma-glutamic acid gel according to claim 4, wherein the enzymatic crosslinking agent is one of horseradish peroxidase and phosphorylase, and the time required for enzymatic crosslinking is 5+/-2 s at 40 ℃.
9. The method for preparing ceramic by casting poly-gamma-glutamic acid gel according to claim 1, wherein the sintering conditions are: the sintering temperature is 1500-1600 ℃ and the sintering time is 1-3 h.
10. The ceramic prepared by the preparation method according to any one of claims 1 to 9 is used as one of a heat insulating ceramic, a wave absorbing ceramic, a biological ceramic, a high temperature ceramic, and a transparent ceramic.
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