CN109267131B - Preparation method of non-combustible material - Google Patents
Preparation method of non-combustible material Download PDFInfo
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- CN109267131B CN109267131B CN201811036958.0A CN201811036958A CN109267131B CN 109267131 B CN109267131 B CN 109267131B CN 201811036958 A CN201811036958 A CN 201811036958A CN 109267131 B CN109267131 B CN 109267131B
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- electrodeposition
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
Abstract
The invention discloses a preparation method of a non-combustible material; the method comprises the following steps: preparing an electrodeposition solution: the solvent in the electrodeposition solution is ethylene glycol, and the solute components and the corresponding molar concentrations are as follows: 0.1-0.2 mol/L of aluminum nitrate and 0.02-0.4 mol/L of zirconium nitrate pentahydrate; respectively taking graphite as a cathode and an anode, and carrying out pulse electrodeposition reaction in an electrodeposition solution to prepare an aluminum-zirconium precursor material; heating the aluminum zirconium precursor material at 200-250 ℃ for 25-50 minutes, and cooling along with the furnace to obtain the aluminum zirconium oxide non-combustible material. The prepared non-combustible material does not contain any organic matter, and the common physical or chemical aging problem of high molecular organic matters can not occur; the material is composed of alumina and zirconia, both of which are high-temperature resistant materials with high chemical stability, the alumina can provide good mechanical strength for the non-combustible material, and meanwhile, the addition of the zirconia can provide certain plasticity for the non-combustible material.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to a preparation method of a non-combustible material.
Background
With the increasing demand for fire safety in public places and domestic houses, the fire resistance of the material is valued by more and more design and construction units and users. Meanwhile, China also promulgates a series of laws and regulations, policy provisions and the like to support the development of fireproof flame-retardant materials which can reach the national fire-fighting standard. Against this background, various novel incombustible sheets have been developed.
Chinese patent publication No. CN103243881B, non-combustible decorative board, discloses a non-combustible decorative board with an inorganic base material containing cement as a main component and an airtight surface decorative layer. Chinese patent No. CN104693632B, A-class non-combustible external wall insulation board, proposes a A-class non-combustible external wall insulation board, which is prepared from 100 parts by weight of polystyrene, 2-3 parts by weight of nucleating agent, 4-7 parts by weight of stabilizer, 47-63 parts by weight of flame retardant, 1-3 parts by weight of foaming agent, 11-15 parts by weight of quaternary cyclopentadienyl tetraol, 2-3% by weight of molybdenum trioxide and 5-7 parts by weight of compatilizer. The composite board recorded in Chinese patent No. CN1073058C, namely inorganic non-combustible composite board, is composed of 90-120 parts of light-burned magnesium oxide, 75-100 parts of magnesium chloride aqueous solution, 5-25 parts of filler, 3-5 parts of water-resistant additive and 5-10 parts of toughening agent. The inorganic non-combustible board recorded in Chinese patent No. CN100408772C 'inorganic non-combustible board and application thereof' has the following composition: 80-130 parts of light-burned magnesia powder; 30-60 parts of halogen sheets; 40-70 parts of water; 5-40 parts of fly ash; 10-30 parts of wood dust; 0-25 parts of expanded perlite; compounding water resisting additive; 0.1-5 parts; 2 layers of glass fiber gridding cloth; 2 layers of non-woven fabric; the composite water-resistant additive is phosphate composite sulfate, and the composite ratio is 1: 9-9: 1; the fly ash is used as an admixture. Chinese patent No. CN100500801C, entitled "non-metal inorganic powder composite non-combustible material and manufacturing method, sheet material and manufacturing method", describes the raw material composition of the composite non-combustible material, which comprises 55-70% of non-metal inorganic powder, 10-30% of adhesive, 10-15% of reinforcing material, 2-4% of auxiliary agent compatilizer and 1-3% of modifier. Chinese patent No. CN104710950B, a "polymer adhesive material for inorganic non-combustible safety-level aluminum composite board" discloses an inorganic non-combustible safety-level aluminum composite board, which is prepared by hot-pressing and continuous composite molding of an aluminum base material, an inorganic core plate and an aluminum base material, wherein the aluminum base material and the inorganic fireproof core layer are bonded by the polymer adhesive material. Chinese patent publication No. CN101870567A, incombustible A2 grade core layer material for fireproof aluminum composite boards and a preparation method thereof, records that the core layer material for incombustible A2 grade fireproof aluminum composite boards is prepared by stirring and mixing 85-95 wt% of inorganic incombustible components, 5-13 wt% of high-molecular adhesive materials and 0.5-5 wt% of auxiliaries.
At present, most of the incombustible plates are prepared by using organic high molecular materials, such as adhesive materials or toughening agents. However, organic polymer materials are prone to physical aging involving changes in molecular conformation and aggregation state structure, such as creep and relaxation, or chemical aging involving changes in molecular structure, such as degradation or crosslinking, under the action of environmental factors, such as light, heat, humidity, stress, corrosive media, etc., thereby causing deterioration in material performance and affecting long-term use of the materials. In addition, the existing preparation process of the non-combustible plate has the problems of complex process and formula, difficult control and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a novel non-combustible material.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a preparation method of a non-combustible material; the preparation method comprises the following steps:
step one, preparing an electrodeposition solution: the solvent in the electrodeposition solution is glycol (the use of glycol in the system of the invention is helpful to form a metal organic complex with the solute, which is convenient for the later electrodeposition process and forms a deposition film layer on the surface of the cathode), and the solute components and the corresponding molar concentrations are as follows: aluminum nitrate (Al (NO)3)3)0.1 to 0.2mol/L of zirconium nitrate (Zr (NO) pentahydrate3)4·5H2O)0.02～0.4mol/L；
Step two, preparing an aluminum zirconium precursor material by electrodeposition: respectively taking graphite as a cathode and an anode, and carrying out pulse electrodeposition reaction in the electrodeposition solution to prepare an aluminum-zirconium precursor material;
step three, preparing the aluminum zirconium oxide non-combustible material: and heating the aluminum zirconium precursor material obtained in the second step at 200-250 ℃ for 25-50 minutes, and cooling along with the furnace to obtain the aluminum zirconium oxide non-combustible material.
Preferably, in the pulse electrodeposition reaction process, the temperature of the electrodeposition solution is controlled to be 20-30 ℃.
Preferably, in the pulse electrodeposition reaction process, the pulse deposition voltage is controlled to be 10-20V, the on-time is 1-2 s, and the off-time is 1 s. And (3) preparing the material by pulse electrodeposition, closing the power supply when the thickness of the material reaches a set value, stopping electrodeposition, taking out the prepared material and cleaning the material by using clear water. The adoption of the pulse electrodeposition mode is beneficial to improving the electrode polarization process in the electrodeposition process, improving the electrodeposition preparation efficiency and improving the performance of the deposited material. If the pulse deposition voltage is higher than 20V, the decomposition reaction of the electrolyte is easy to occur, and the electro-deposition preparation of the material cannot be realized; if the pulse deposition voltage is lower than 10V, the preparation efficiency of the material is too low and the material cannot form a continuous compact structure.
Preferably, in the pulse electrodeposition reaction process, the distance between the cathode and the anode is 5-10 cm.
Preferably, the second step is specifically: injecting the electrodeposition solution of the first step into an electrodeposition bath; putting graphite as a cathode into an electrodeposition tank, and putting the other graphite as an anode into the electrodeposition tank; the cathode is in full contact with the electrodeposition solution in the electrodeposition tank while avoiding the contact of the cathode with the anode, and the cathode and the anode are connected with a pulse power supply to form a loop.
Compared with the prior art, the invention has the following beneficial effects:
1. the non-combustible material prepared by the method is an inorganic composite oxide material and does not contain any organic matter, so that the common physical or chemical aging problem of high molecular organic matters is avoided;
2. the aluminum-zirconium oxide non-combustible material provided by the invention consists of alumina and zirconia, wherein the alumina and the zirconia are both high-temperature-resistant materials with high chemical stability, the alumina can provide good mechanical strength for the non-combustible material, and meanwhile, the addition of the zirconia can provide certain plasticity for the non-combustible material, so that the aluminum-zirconium oxide non-combustible material has important significance for the practical application of the non-combustible material.
3. The process formula is simple, the formula of the electrodeposition solution related by the invention only has two solutes, and the material preparation process also only comprises two steps;
4. the invention is based on the preparation of the material by the electrodeposition and the subsequent heat treatment methods, impurities are not easy to be introduced in the preparation process, and the invention has the advantage of high material purity;
5. in addition, the content of elements in the noncombustible material can be adjusted by changing the formulation of the electrodeposition solution.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment relates to a preparation method of a non-combustible material; the preparation method comprises the following steps:
step one, preparing an electrodeposition solution: the solvent in the electrodeposition solution is ethylene glycol, and the solute components and the corresponding molar concentrations are as follows: aluminum nitrate (Al (NO)3)3)0.15mol/L, zirconium nitrate pentahydrate (Zr (NO)3)4·5H2O)0.2mol/L；
Step two, preparing an aluminum zirconium precursor material by electrodeposition: injecting the electrodeposition solution of the first step into an electrodeposition bath; putting graphite as a cathode into an electrodeposition tank, and putting graphite as an anode into the electrodeposition tank; the cathode is fully contacted with the electrodeposition solution in the electrodeposition tank, meanwhile, the cathode is prevented from being contacted with the anode (the distance between the cathode and the anode is controlled to be 5-10 cm, in the embodiment, 8cm), and the cathode and the anode are connected with a pulse power supply to form a loop; controlling the temperature of the electrodeposition solution to be 25 ℃, controlling the pulse deposition voltage to be 15V, the on-time to be 1.5s and the off-time to be 1s, and performing pulse electrodeposition to prepare an aluminum-zirconium precursor material (specifically, depositing the material on the surface of a cathode); when the thickness of the material reaches a set value, turning off the power supply, stopping the electrodeposition, taking out the prepared material and cleaning the material by using clear water;
step three, preparing the aluminum zirconium oxide non-combustible material: and heating the aluminum zirconium precursor material obtained in the second step at 225 ℃ for 40 minutes, and then cooling along with the furnace to obtain the aluminum zirconium oxide non-combustible material. The finally prepared aluminum zirconium oxide non-combustible material is shown by inductively coupled plasma mass spectrometry to comprise the following elements in percentage by weight: aluminum: 62%, zirconium: 38 percent.
Example 2
The embodiment relates to a preparation method of a non-combustible material; the preparation method is basically the same as that of the example 1; the difference lies in that:
in the first step, the components of the solute in the electrodeposition solution and the corresponding molar concentrations are: mirabiliteAluminum (Al (NO)3)3)0.1mol/L, zirconium nitrate pentahydrate (Zr (NO)3)4·5H2O)0.02mol/L；
In the second step, the temperature of the electrodeposition solution is controlled to be 20 ℃, the pulse deposition voltage is controlled to be 20V, the on-time is 1s, and the off-time is 1 s;
in the third step, the aluminum zirconium precursor material obtained in the second step is heated at 250 ℃ for 25 minutes. The finally prepared aluminum zirconium oxide non-combustible material is shown by inductively coupled plasma mass spectrometry to comprise the following elements in percentage by weight: aluminum: 83%, zirconium: 17 percent.
Example 3
The embodiment relates to a preparation method of a non-combustible material; the preparation method is basically the same as that of the example 1; the difference lies in that:
in the first step, the components of the solute in the electrodeposition solution and the corresponding molar concentrations are: aluminum nitrate (Al (NO)3)3)0.2mol/L, zirconium nitrate pentahydrate (Zr (NO)3)4·5H2O)0.4mol/L；
In the second step, the temperature of the electrodeposition solution is controlled to be 30 ℃, the pulse deposition voltage is controlled to be 10V, the on-time is 2s, and the off-time is 1 s;
in the third step, the aluminum zirconium precursor material obtained in the second step is heated for 50 minutes at 200 ℃. The finally prepared aluminum zirconium oxide non-combustible material is shown by inductively coupled plasma mass spectrometry to comprise the following elements in percentage by weight: aluminum: 55%, zirconium: 45 percent.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (3)
1. A method for producing a noncombustible material, characterized by comprising the steps of:
step one, preparing an electrodeposition solution: the solvent in the electrodeposition solution is ethylene glycol, and the solute components and the corresponding molar concentrations are as follows: 0.1-0.2 mol/L of aluminum nitrate and 0.02-0.4 mol/L of zirconium nitrate pentahydrate;
step two, preparing an aluminum zirconium precursor material by electrodeposition: graphite is respectively used as a cathode and an anode, pulse electrodeposition reaction is carried out in the electrodeposition solution, and an aluminum-zirconium precursor material is prepared by deposition on the surface of the cathode; in the pulse electrodeposition reaction process, controlling the pulse deposition voltage to be 10-20V, the on-time to be 1-2 s and the off-time to be 1 s;
step three, preparing the aluminum zirconium oxide non-combustible material: and heating the aluminum zirconium precursor material obtained in the second step at 200-250 ℃ for 25-50 minutes, and cooling along with the furnace to obtain the aluminum zirconium oxide non-combustible material.
2. The method for preparing a noncombustible material according to claim 1, wherein the temperature of the electrodeposition solution is controlled to 20 to 30 ℃ during the pulse electrodeposition reaction.
3. The method for preparing a noncombustible material according to claim 1, wherein a distance between the cathode and the anode during the pulse electrodeposition reaction is 5 to 10 cm.
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| CN201811036958.0A CN109267131B (en) | 2018-09-06 | 2018-09-06 | Preparation method of non-combustible material |
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| CN201811036958.0A CN109267131B (en) | 2018-09-06 | 2018-09-06 | Preparation method of non-combustible material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220248A (en) * | 1997-12-19 | 1999-06-23 | 化学工业部天津化工研究院 | Method for preparing zirconium oxide-aluminum oxide composite and its use |
| CN101233083A (en) * | 2005-08-25 | 2008-07-30 | 赢创德固赛有限责任公司 | Stabilised aluminium zirconium mixed oxide powder |
| CN104562128A (en) * | 2015-01-09 | 2015-04-29 | 西安工业大学 | Method for preparing thermal protection ceramic layer on surface of metal or metal composite material |
| CN104911662A (en) * | 2012-05-10 | 2015-09-16 | 中国兵器工业第五九研究所 | Preparation method of composite ceramic coating layer |
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2018
- 2018-09-06 CN CN201811036958.0A patent/CN109267131B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1220248A (en) * | 1997-12-19 | 1999-06-23 | 化学工业部天津化工研究院 | Method for preparing zirconium oxide-aluminum oxide composite and its use |
| CN101233083A (en) * | 2005-08-25 | 2008-07-30 | 赢创德固赛有限责任公司 | Stabilised aluminium zirconium mixed oxide powder |
| CN104911662A (en) * | 2012-05-10 | 2015-09-16 | 中国兵器工业第五九研究所 | Preparation method of composite ceramic coating layer |
| CN104562128A (en) * | 2015-01-09 | 2015-04-29 | 西安工业大学 | Method for preparing thermal protection ceramic layer on surface of metal or metal composite material |
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