CN103274617A - Aluminum dihydrogen phosphate nano/micro-binder and preparation method thereof - Google Patents
Aluminum dihydrogen phosphate nano/micro-binder and preparation method thereof Download PDFInfo
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- CN103274617A CN103274617A CN2013101507625A CN201310150762A CN103274617A CN 103274617 A CN103274617 A CN 103274617A CN 2013101507625 A CN2013101507625 A CN 2013101507625A CN 201310150762 A CN201310150762 A CN 201310150762A CN 103274617 A CN103274617 A CN 103274617A
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Abstract
The invention provides an aluminum dihydrogen phosphate nano/micro-binder and a preparation method thereof. The aluminum dihydrogen phosphate nano/micro-binder comprises, by weight, 50 to 80% of aluminum dihydrogen phosphate colloid and 20 to 50% of aluminum dihydrogen phosphate nano/micro-particles. The aluminum dihydrogen phosphate colloid comprises, by weight, 10 to 20% of aluminum hydroxide, 40 to 85% of phosphoric acid and 10 to 20% of water. A preparation method of the aluminum dihydrogen phosphate colloid comprises that aluminum hydroxide, phosphoric acid and water are mixed uniformly according to the above ratio and then undergo a reaction at a temperature of 85 to 100 DEG C under the heating condition for 1 to 2h. The aluminum dihydrogen phosphate nano/micro-particles are prepared by template-based guiding of the aluminum dihydrogen phosphate colloid. A preparation method of the aluminum dihydrogen phosphate nano/micro-particles comprises reaction and curing processes. The aluminum dihydrogen phosphate nano/micro-particles have particle sizes of 100 nanometers to 1 micron. The aluminum dihydrogen phosphate colloid and the aluminum dihydrogen phosphate nano/micro-particles are mixed uniformly into the aluminum dihydrogen phosphate nano/micro-binder according to a certain ratio by a mechanical mixing method. The aluminum dihydrogen phosphate nano/micro-binder can be used in a high temperature-resistant coating mater and a high-temperature refractory material, and has excellent cohesiveness in a high-temperature environment.
Description
Technical field
The present invention relates to the binder material field, especially a kind of aluminium dihydrogen phosphate for high temperature material is received little binding agent and preparation method thereof.
Background technology
The biphosphate al binder is because bonding, casting, grinding tool and the military field that the bonding scope is wide, the cohesive strength advantages of higher is widely used in refractory materials in coating, the high temperature kiln, maintenance of equipment and sealing modification, pottery and ceramic composite.At present also use the biphosphate al binder in a lot of coated materials, but received the unique effect that realizes nano-micro structure in the micron coating often by a large amount of inorganic nano-particle of adding.Introduce from the angle of binding agent and to receive micropartical, be conducive to significantly improve the adhesive property of binding agent, improve the granularity coupling of coating, so that better effect of protective coating performance.
Chinese patent CN101426872B discloses a kind of high temperature resistant inorganic composite adhesive, and the composition of binding agent comprises 5%～12% aluminium hydroxide, 15～35% phosphoric acid, 0.1～1% rare earth oxide, 5～20% silicon sol, 1～15% polyphosphoric acid aluminium, 1～5% borax and the water of surplus.The characteristics of this binding agent are to be used for metal works thermal treatment temporary protection coatings such as high-temperature coatings and high-temperature oxidation resistant coating; can realize that coating is directly 400～1000 ℃ of hot metal matrix surface sprayings; and under hot environment, can keep high adhesive property; but its consumption accounts for 10%～20% of high temperature resistant powder, large usage quantity.
The production method of present nanoparticle has a variety of, comprises hydrothermal method, sol-gel method, mechanical ball milling method, chemical Vapor deposition process etc., and the common issue with that these methods exist is that the material preparation cost is higher, has limited the application of nanoparticle.Therefore developing the lower microstage mineral binder bond of receiving of preparation cost has important practical significance.
Summary of the invention
The technical problem underlying that the present invention solves is to provide a kind of aluminium dihydrogen phosphate to receive little binding agent and preparation method thereof, and this binding agent can be used in coated material and the refractory materials, has good adhesive property under hot environment.
The invention provides a kind of aluminium dihydrogen phosphate and receive little binding agent, described binding agent is made of by weight percentage following composition: 50%～80% aluminium dihydrogen phosphate colloid, 20%～50% aluminum phosphate are received micropartical; Described aluminium dihydrogen phosphate colloid according to chemical composition is made up of aluminium hydroxide 10%～20%, phosphatase 24 0%～85% and water 10%～20%, and the preparation method reacts 1～2h for phosphoric acid, aluminium hydroxide and water are mixed in proportion under 85～100 ℃ of heating conditions.The described micropartical of receiving is that the aluminium dihydrogen phosphate colloid forms through the template guiding, mainly comprises reaction and maturing process, and the made micropartical of receiving is of a size of 100nm～1 μ m, and its main preparation process is as follows:
1) configuration concentration is the aluminium dihydrogen phosphate colloidal solution of 20g/L;
2) add the template of 0.5～25g/L in the above-mentioned solution, stir;
3) will add the aluminium dihydrogen phosphate colloidal solution sealing of template, and be placed under 60～100 ℃ the condition and react 10～24h;
4) throw out that the step 3) reaction is obtained filters, and uses distilled water wash 3 times;
5) throw out after will washing was placed on curing in water 1～15 day, and ambient temperature is 25 ℃;
6) with behind the usefulness distilled water of the throw out after the slaking and the absolute ethanol washing, after the vacuum drying oven drying, obtain target product aluminum phosphate nanoparticle.
With aluminium dihydrogen phosphate colloid and aluminum phosphate nanoparticle in proportion (50%～80% aluminium dihydrogen phosphate colloid, 20%～50% aluminum phosphate receive micropartical) mix with mechanical mixing and obtain aluminium dihydrogen phosphate and receive little binding agent.
Used template is that template is a kind of or its combination in fluorine hydrogenation ammonia, primary ammonium phosphate, the thionamic acid ammonia among the present invention.Usually under the effect of fluorine hydrogenation ammonia template, it is spherical or rectangular flap that aluminum phosphate is received atomic proterties, and along with the increase of template concentration, the atomic shape of receiving is tended to and spherical shape becomes rectangular sheet, and the thickness of rectangular sheet is 200～500nm.Under the effect of thionamic acid ammonia template, receive the atomic roundel that is shaped as, disk thickness is 100～300nm.Under the effect of primary ammonium phosphate template, to receive and atomicly be shaped as cylindricly, the diameter of cylinder bottom surface is 100nm～200nm, is about 500nm～1 μ m.
Positively effect of the present invention is:
1. the binding agent among the present invention has added and has received micropartical, and it is lower to receive atomic preparation cost, and preparation condition is simpler.
2. the aluminium dihydrogen phosphate among the present invention is received little binding agent and be can be used in present high-temperature coatings and the refractory materials, receives the mutual chimeric raising that helps adhesion strength of micropartical and powder aggregate, and binding agent still has the good adhesive force performance in heat-processed.
3. the aluminium dihydrogen phosphate among the present invention is received little binding agent owing to contain and is received micropartical, and consumption accounts in high temperature coating material and refractory materials 1%～10%.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Get 10% aluminium hydroxide, 10% water and 80% phosphoric acid, mix the back and under 85～100 ℃ of heating conditions, react 2h, obtain aluminium dihydrogen phosphate colloid A, colloid A is mixed with the aluminium dihydrogen phosphate colloidal solution of 20g/L, the fluorine hydrogenation ammonia of the ammonium chloride of adding 20g/L and 0.5g/L is as template in above-mentioned solution, place then under 80 ℃ the condition and react 24h, to be placed on curing in water 10 days after the product washing, ambient temperature is 25 ℃, behind the usefulness distilled water of the throw out after the slaking and absolute ethanol washing, obtain the aluminum phosphate nanoparticle after the vacuum drying oven drying, receive the atomic rectangular sheet that is shaped as, rectangular thickness is 300nm.20% the micropartical of receiving is added among 80% the aluminium dihydrogen phosphate colloid A, obtain aluminium dihydrogen phosphate through mechanically mixing and receive little binding agent.
Embodiment 2
Get 20% aluminium hydroxide, 10% water and 70% phosphoric acid, mix the back and under 85～100 ℃ of heating conditions, react 1.5h, obtain aluminium dihydrogen phosphate colloid B, colloid B is mixed with the aluminium dihydrogen phosphate colloidal solution of 20g/L, in above-mentioned solution, add the primary ammonium phosphate of 1g/L as template, place then under 90 ℃ the condition and react 24h, to be placed on curing in water 7 days after the product washing, ambient temperature is 25 ℃, throw out after the slaking with behind distilled water and the absolute ethanol washing, is obtained the aluminum phosphate nanoparticle after the vacuum drying oven drying, receive atomic be shaped as cylindric, the diameter of cylinder bottom surface is 150nm, is about 800nm.30% the micropartical of receiving is added among 70% the aluminium dihydrogen phosphate colloid B, obtain aluminium dihydrogen phosphate through mechanically mixing and receive little binding agent.
Embodiment 3
Get 20% aluminium hydroxide, 20% water and 60% phosphoric acid, mix the back and under 85～100 ℃ of heating conditions, react 1h, obtain aluminium dihydrogen phosphate colloid C, colloid C is mixed with the aluminium dihydrogen phosphate colloidal solution of 20g/L, the thionamic acid ammonia of adding 5g/L and 1g/L hydrogen fluoride ammonia are as template in above-mentioned solution, place then under 100 ℃ the condition and react 24h, to be placed on curing in water 15 days after the product washing, ambient temperature is 25 ℃, behind the usefulness distilled water of the throw out after the slaking and absolute ethanol washing, obtain the aluminum phosphate nanoparticle after the vacuum drying oven drying, receive the atomic roundel that is shaped as, disk thickness is 100～300nm
40% the micropartical of receiving is added among 60% the aluminium dihydrogen phosphate colloid C, obtain aluminium dihydrogen phosphate through mechanically mixing and receive little binding agent.
The aluminium dihydrogen phosphate of making according to above each embodiment and method is received little binding agent and is applicable in the high-temperature coatings, has excellent cohesive strength, high temperature moment adhesion strength reaches 0.3～0.5MPa, and aluminium dihydrogen phosphate is received after little binding agent joins coating, and the barrier propterty of coating is significantly improved.The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (4)
1. an aluminium dihydrogen phosphate is received little binding agent, it is characterized in that, by 50%～80% aluminium dihydrogen phosphate colloid and 20%～50% aluminum phosphate nanoparticle by weight percentage mechanically mixing form, the aluminium dihydrogen phosphate colloid is according to chemical composition made under 85～100 ℃ heating condition by aluminium hydroxide 10%～20%, phosphoric acid 60%～80% and water 10%～20%.
2. an aluminium dihydrogen phosphate is received the preparation method of little binding agent, it is characterized in that its preparation process is as follows:
1) configuration concentration is the aluminium dihydrogen phosphate colloidal solution of 20g/L;
2) add the template of 0.5～20g/L in the above-mentioned solution, stir;
3) will add the aluminium dihydrogen phosphate colloidal solution sealing of template, and be placed under 60～100 ℃ the condition and react 10～24h;
4) throw out that the step 3) reaction is obtained filters, and uses distilled water wash 3 times;
5) throw out after will washing was placed on curing in water 1～15 day, and ambient temperature is 25 ℃;
6) with behind the usefulness distilled water of the throw out after the slaking and the absolute ethanol washing, after the vacuum drying oven drying, obtain target product aluminum phosphate nanoparticle.
3. aluminium dihydrogen phosphate according to claim 1 is received little binding agent, it is characterized in that, the described micropartical of receiving is a kind of or its combination of the aluminum phosphate globe that is of a size of 100nm～1 μ m, aluminum phosphate cylinder, the rectangular flap of aluminum phosphate.
4. aluminium dihydrogen phosphate according to claim 2 is received the preparation method of little binding agent, it is characterized in that described template is a kind of or its combination in fluorine hydrogenation ammonia, primary ammonium phosphate, the thionamic acid ammonia.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103762013A (en) * | 2013-12-31 | 2014-04-30 | 宁波兴慈热动电器有限公司 | High-temperature insulation material for electronic heater and preparation method |
| CN104762020A (en) * | 2015-04-07 | 2015-07-08 | 唐山学院 | Method for preparing refractory material adhesive from oxidized wastewater sludge in aluminum alloy section plants |
| CN108088792A (en) * | 2017-11-27 | 2018-05-29 | 中国船舶重工集团公司第七二五研究所 | Dirty sample and preparation method and application among a kind of |
| CN108793117A (en) * | 2018-09-18 | 2018-11-13 | 湖北武洲新材料科技有限公司 | A kind of micro- binder stand-by provision of aluminium dihydrogen phosphate sodium |
| CN110511682A (en) * | 2018-05-22 | 2019-11-29 | 天津大学（青岛）海洋工程研究院有限公司 | A kind of high universalizable phosphalugel adhesive resistant to high temperature and preparation method thereof |
| CN112687445A (en) * | 2021-01-20 | 2021-04-20 | 合肥工业大学 | Preparation method of aluminum dihydrogen phosphate-based composite insulation coated metal soft magnetic powder core |
| CN115433479A (en) * | 2022-10-18 | 2022-12-06 | 中国民航大学 | Preparation method of phosphate gum base flame-retardant heat-insulating coating highly ceramic when encountering fire |
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| CN85100057A (en) * | 1985-04-01 | 1986-07-23 | 清华大学 | High-temperature strain sustainable adhesive |
| CN86106831A (en) * | 1985-09-10 | 1987-03-11 | 卡尔文·舒鲍 | The combination material of fire prevention and insulation usefulness |
| CN101037194A (en) * | 2003-03-14 | 2007-09-19 | 日本化学工业株式会社 | High purity metaphosphate and its production method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN85100057A (en) * | 1985-04-01 | 1986-07-23 | 清华大学 | High-temperature strain sustainable adhesive |
| CN86106831A (en) * | 1985-09-10 | 1987-03-11 | 卡尔文·舒鲍 | The combination material of fire prevention and insulation usefulness |
| CN101037194A (en) * | 2003-03-14 | 2007-09-19 | 日本化学工业株式会社 | High purity metaphosphate and its production method |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103762013A (en) * | 2013-12-31 | 2014-04-30 | 宁波兴慈热动电器有限公司 | High-temperature insulation material for electronic heater and preparation method |
| CN103762013B (en) * | 2013-12-31 | 2016-05-11 | 宁波兴慈热动电器有限公司 | A kind of electronic heater high temperature insulating material and preparation method |
| CN104762020A (en) * | 2015-04-07 | 2015-07-08 | 唐山学院 | Method for preparing refractory material adhesive from oxidized wastewater sludge in aluminum alloy section plants |
| CN104762020B (en) * | 2015-04-07 | 2016-08-17 | 唐山学院 | The method preparing fire bond with aluminium alloy extrusions factory oxidized waste water mud |
| CN108088792A (en) * | 2017-11-27 | 2018-05-29 | 中国船舶重工集团公司第七二五研究所 | Dirty sample and preparation method and application among a kind of |
| CN110511682A (en) * | 2018-05-22 | 2019-11-29 | 天津大学（青岛）海洋工程研究院有限公司 | A kind of high universalizable phosphalugel adhesive resistant to high temperature and preparation method thereof |
| CN108793117A (en) * | 2018-09-18 | 2018-11-13 | 湖北武洲新材料科技有限公司 | A kind of micro- binder stand-by provision of aluminium dihydrogen phosphate sodium |
| CN112687445A (en) * | 2021-01-20 | 2021-04-20 | 合肥工业大学 | Preparation method of aluminum dihydrogen phosphate-based composite insulation coated metal soft magnetic powder core |
| CN115433479A (en) * | 2022-10-18 | 2022-12-06 | 中国民航大学 | Preparation method of phosphate gum base flame-retardant heat-insulating coating highly ceramic when encountering fire |
| CN115433479B (en) * | 2022-10-18 | 2023-06-27 | 中国民航大学 | Preparation method of phosphate gum base flame-retardant heat-insulating coating with high ceramization degree in fire |
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