CN103274617B - A kind of Aluminum dihydrogen phosphate nano/micro-binder and preparation method thereof - Google Patents
A kind of Aluminum dihydrogen phosphate nano/micro-binder and preparation method thereof Download PDFInfo
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- CN103274617B CN103274617B CN201310150762.5A CN201310150762A CN103274617B CN 103274617 B CN103274617 B CN 103274617B CN 201310150762 A CN201310150762 A CN 201310150762A CN 103274617 B CN103274617 B CN 103274617B
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Abstract
The invention provides a kind of Aluminum dihydrogen phosphate nano/micro-binder and preparation method thereof, described binding agent is made up of by weight percentage following composition: 50 ~ 80% aluminium dihydrogen phosphate colloids, and micropartical received by 20 ~ 50% aluminum phosphates.Described aluminium dihydrogen phosphate colloid is according to chemical composition made up of aluminium hydroxide 10% ~ 20%, phosphatase 24 0% ~ 85% and water 105 ~ 20%, and preparation method, for phosphoric acid, aluminium hydroxide and water to be mixed in proportion, reacts 1 ~ 2h under 85 ~ 100 DEG C of heating conditions.Described micropartical of receiving is that aluminium dihydrogen phosphate colloid is formed through template guiding, and mainly comprise reaction and maturing process, made micropartical of receiving is of a size of 100nm ~ 1 μm.Aluminium dihydrogen phosphate colloid and aluminum phosphate nanoparticle are mixed with mechanical mixing in proportion and obtains Aluminum dihydrogen phosphate nano/micro-binder.Aluminum dihydrogen phosphate nano/micro-binder of the present invention can be used in high temperature-resistant coating material and high-temperature refractory, has excellent adhesive property in high temperature environments.
Description
Technical field
The present invention relates to binder material field, especially a kind of Aluminum dihydrogen phosphate nano/micro-binder for high temperature material and preparation method thereof.
Background technology
Biphosphate al binder because bonding scope is wide, cohesive strength advantages of higher is widely used in refractory materials in coating, high temperature kiln, maintenance of equipment and sealing is modified, the bonding of pottery and ceramic composite, casting, grinding tool and military field.Also used biphosphate al binder in a lot of coated material at present, but received in micron coating often by adding a large amount of inorganic nano-particles to realize the unique effect of nano-micro structure.Introduce from the angle of binding agent and receive micropartical, be conducive to the adhesive property significantly improving binding agent, improve the particle size matching of coating, so that protective coating plays better effect.
Chinese patent CN101426872B discloses a kind of high temperature resistant inorganic composite adhesive, the composition of binding agent comprise 5% ~ 12% aluminium hydroxide, 15 ~ 35% phosphoric acid, 0.1 ~ 1% rare earth oxide, 5 ~ 20% silicon sol, 1 ~ 15% polyphosphoric acid aluminium, the borax of 1 ~ 5% and the water of surplus.The feature of this binding agent is to be used in the metal works such as high-temperature coatings and high-temperature oxidation resistant coating thermal treatment temporary protection coating; coating can be realized directly 400 ~ 1000 DEG C of hot metal matrix surface sprayings; and excellent adhesive property can be kept in high temperature environments; but its consumption accounts for 10% ~ 20% of high temperature resistant powder, large usage quantity.
The production method of current nanoparticle has a variety of, comprises hydrothermal method, sol-gel method, mechanical attrition method, chemical Vapor deposition process etc., and the common issue that these methods exist is that material preparation cost is higher, limits the application of nanoparticle.Therefore the microstage mineral binder bond of receiving developing preparation cost lower has important practical significance.
Summary of the invention
The technical problem underlying that the present invention solves is to provide a kind of Aluminum dihydrogen phosphate nano/micro-binder and preparation method thereof, and this binding agent can be used for, in coated material and refractory materials, having good adhesive property in high temperature environments.
The invention provides a kind of Aluminum dihydrogen phosphate nano/micro-binder, described binding agent is made up of by weight percentage following composition: 50% ~ 80% aluminium dihydrogen phosphate colloid, and micropartical received by 20% ~ 50% aluminum phosphate; Described aluminium dihydrogen phosphate colloid is according to chemical composition made up of aluminium hydroxide 10% ~ 20%, phosphatase 24 0% ~ 85% and water 10% ~ 20%, and preparation method, for phosphoric acid, aluminium hydroxide and water to be mixed in proportion, reacts 1 ~ 2h under 85 ~ 100 DEG C of heating conditions.Described micropartical of receiving is that aluminium dihydrogen phosphate colloid is formed through template guiding, and mainly comprise reaction and maturing process, made micropartical of receiving is of a size of 100nm ~ 1 μm, and its main preparation process is as follows:
1) configuration concentration is the aluminium dihydrogen phosphate colloidal solution of 20g/L;
2) in above-mentioned solution, add the template of 0.5 ~ 25g/L, stir;
3) the aluminium dihydrogen phosphate colloidal solution sealing of template will be added, under being placed on the condition of 60 ~ 100 DEG C, react 10 ~ 24h;
4) throw out that step 3) is obtained by reacting filters, with distilled water wash 3 times;
5) throw out after washing is placed on curing in water 1 ~ 15 day, ambient temperature is 25 DEG C;
6) by after the throw out distilled water after slaking and absolute ethanol washing, after vacuum drying oven drying, target product aluminum phosphate nanoparticle is obtained.
By aluminium dihydrogen phosphate colloid and aluminum phosphate nanoparticle in proportion (50% ~ 80% aluminium dihydrogen phosphate colloid, 20% ~ 50% aluminum phosphate receive micropartical) to mix with mechanical mixing and obtain Aluminum dihydrogen phosphate nano/micro-binder.
Template used in the present invention one that to be template be in fluorine hydrogenation ammonia, primary ammonium phosphate, thionamic acid ammonia or its combination.Usually under the effect of fluorine hydrogenation ammonia template, atomic proterties received by aluminum phosphate is spherical or rectangular flap, and along with the increase of template concentration, 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, atomic shape of receiving is roundel, and wafer thickness is 100 ~ 300nm.Under the effect of primary ammonium phosphate template, atomic shape of receiving is cylindric, and the diameter of bottom cylindrical face is 100nm ~ 200nm, is about 500nm ~ 1 μm.
Positively effect of the present invention is:
1. the binding agent in the present invention with the addition of receives micropartical, and it is lower to receive atomic preparation cost, and preparation condition is simpler.
2. the Aluminum dihydrogen phosphate nano/micro-binder in the present invention can be used in current high-temperature coatings and refractory materials, receives the mutually chimeric raising contributing to adhesion strength of micropartical and powder aggregate, and binding agent still has good adhesion property in heat-processed.
3. the Aluminum dihydrogen phosphate nano/micro-binder in the present invention due to containing receiving micropartical, in high temperature coating material and refractory materials, consumption accounts for 1% ~ 10%.
Embodiment
Below embodiments of the invention are elaborated: the present embodiment is implemented under premised on technical solution of the present invention, give 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, under 85 ~ 100 DEG C of heating conditions, 2h is reacted after mixing, 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 and 0.5g/L that add 20g/L in above-mentioned solution is as template, then 24h is reacted under being placed in the condition of 80 DEG C, curing in water is placed on 10 days after being washed by product, ambient temperature is 25 DEG C, after the throw out distilled water after slaking and absolute ethanol washing, aluminum phosphate nanoparticle is obtained after vacuum drying oven drying, atomic shape of receiving is rectangular sheet, the thickness of rectangular is 300nm.The micropartical of receiving of 20% is added in the aluminium dihydrogen phosphate colloid A of 80%, obtains Aluminum dihydrogen phosphate nano/micro-binder through mechanically mixing.
Embodiment 2
Get 20% aluminium hydroxide, 10% water and 70% phosphoric acid, under 85 ~ 100 DEG C of heating conditions, 1.5h is reacted after mixing, obtain aluminium dihydrogen phosphate colloid B, colloid B is mixed with the aluminium dihydrogen phosphate colloidal solution of 20g/L, the primary ammonium phosphate of 1g/L is added as template in above-mentioned solution, then 24h is reacted under being placed in the condition of 90 DEG C, curing in water is placed on 7 days after being washed by product, ambient temperature is 25 DEG C, after the throw out distilled water after slaking and absolute ethanol washing, aluminum phosphate nanoparticle is obtained after vacuum drying oven drying, atomic shape of receiving is cylindric, the diameter of bottom cylindrical face is 150nm, be about 800nm.The micropartical of receiving of 30% is added in the aluminium dihydrogen phosphate colloid B of 70%, obtains Aluminum dihydrogen phosphate nano/micro-binder through mechanically mixing.
Embodiment 3
Get 20% aluminium hydroxide, 20% water and 60% phosphoric acid, under 85 ~ 100 DEG C of heating conditions, 1h is reacted after mixing, 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 5g/L and 1g/L hydrogen fluoride ammonia is added as template in above-mentioned solution, then 24h is reacted under being placed in the condition of 100 DEG C, curing in water is placed on 15 days after being washed by product, ambient temperature is 25 DEG C, after the throw out distilled water after slaking and absolute ethanol washing, aluminum phosphate nanoparticle is obtained after vacuum drying oven drying, atomic shape of receiving is roundel, wafer thickness is 100 ~ 300nm
The micropartical of receiving of 40% is added in the aluminium dihydrogen phosphate colloid C of 60%, obtains Aluminum dihydrogen phosphate nano/micro-binder through mechanically mixing.
Be applicable in high-temperature coatings according to the Aluminum dihydrogen phosphate nano/micro-binder that above each embodiment and method make, there is excellent cohesive strength, high temperature moment adhesion strength reaches 0.3 ~ 0.5MPa, and after Aluminum dihydrogen phosphate nano/micro-binder joins coating, the barrier propterty of coating is significantly improved.The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the preparation method of an Aluminum dihydrogen phosphate nano/micro-binder, it is characterized in that, by 50% ~ 80% aluminium dihydrogen phosphate colloid and 20% ~ 50% aluminum phosphate nanoparticle by weight percentage mechanically mixing form, aluminium dihydrogen phosphate colloid is according to chemical composition made under the heating condition of 85 ~ 100 DEG C by aluminium hydroxide 10% ~ 20%, phosphoric acid 60% ~ 80% and water 10% ~ 20%, described nanoparticle is of a size of the aluminum phosphate globe of 100nm ~ 1 μm, aluminum phosphate cylinder, the one of the rectangular flap of aluminum phosphate or its combination, and its aluminum phosphate nanoparticle preparation process is as follows:
1) configuration concentration is the aluminium dihydrogen phosphate colloidal solution of 20g/L;
2) in above-mentioned solution, add the template of 0.5 ~ 20g/L, stir;
3) the aluminium dihydrogen phosphate colloidal solution sealing of template will be added, under being placed on the condition of 60 ~ 100 DEG C, react 10 ~ 24h;
4) throw out that step 3) is obtained by reacting filters, with distilled water wash 3 times;
5) throw out after washing is placed on curing in water 1 ~ 15 day, ambient temperature is 25 DEG C;
6) by after the throw out distilled water after slaking and absolute ethanol washing, after vacuum drying oven drying, target product aluminum phosphate nanoparticle is obtained.
2. the preparation method of a kind of Aluminum dihydrogen phosphate nano/micro-binder according to claim 1, is characterized in that, described template is one in fluorine hydrogenation ammonia, primary ammonium phosphate, thionamic acid ammonia or its combination.
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| 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 |
| 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 |
| CN108088792B (en) * | 2017-11-27 | 2021-04-02 | 中国船舶重工集团公司第七二五研究所 | Intermediate scale sample and preparation method and application thereof |
| 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 |
| CN108793117B (en) * | 2018-09-18 | 2020-06-19 | 湖北武洲新材料科技有限公司 | Device for preparing sodium aluminum dihydrogen phosphate micro-binder |
| CN112687445B (en) * | 2021-01-20 | 2022-08-30 | 合肥工业大学 | Preparation method of aluminum dihydrogen phosphate-based composite insulation coated metal soft magnetic powder core |
| 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 |
| CN115747485A (en) * | 2022-12-13 | 2023-03-07 | 建平天正矿业有限公司 | A metallurgical pellet bentonite bonding enhancer compound and its application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85100057A (en) * | 1985-04-01 | 1986-07-23 | 清华大学 | High Temperature Strain Adhesive |
| CN86106831A (en) * | 1985-09-10 | 1987-03-11 | 卡尔文·舒鲍 | Composite materials for fire protection and insulation |
| 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 |
|---|---|---|---|---|
| CN85100057A (en) * | 1985-04-01 | 1986-07-23 | 清华大学 | High Temperature Strain Adhesive |
| CN86106831A (en) * | 1985-09-10 | 1987-03-11 | 卡尔文·舒鲍 | Composite materials for fire protection and insulation |
| 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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