CN107974105A - A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating - Google Patents
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating Download PDFInfo
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- CN107974105A CN107974105A CN201711033188.XA CN201711033188A CN107974105A CN 107974105 A CN107974105 A CN 107974105A CN 201711033188 A CN201711033188 A CN 201711033188A CN 107974105 A CN107974105 A CN 107974105A
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- stannic oxide
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2231—Oxides; Hydroxides of metals of tin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention discloses a kind of preparation method of the doping vario-property stannic oxide for glass heat-insulating coating, using hydro-thermal method by the manganese in manganese sulfate monohydrate, ammonium fluoride, Fluorin doped in stannic oxide, control suitable hydrothermal temperature and time, so that the crystallinity of crystal is gradually perfect, stannic oxide through overdoping has superior photoelectric properties, there is selectivity well to solar spectrum, there is good permeability to visible ray, it is infrared to have very strong reflectivity；Then under the action of polyethylene of dispersing agent pyrrolidones, grinding has the near-infrared radiation in sunlight obvious absorption and scattering with obtaining the lanthanum hexaboride slurry of Nano grade under supersonic synergetic effect；It is spray-dried after finally doping vario-property stannic oxide is compounded with nanometer lanthanum hexaboride, obtained product particle is fine and smooth, it can be added to as filler in macromolecule matrix, can be compatible and be uniformly dispersed well with macromolecule matrix, heat insulation is excellent and stability is good.
Description
Technical field
The present invention relates to insulating moulding coating technical field, more particularly to a kind of doping vario-property dioxy for glass heat-insulating coating
Change the preparation method of tin.
Background technology
In recent years, energy shortage situation is increasingly taken seriously, and China is the country of a high energy consumption, solves energy crisis
Not only stop in terms of exploring novel energy, it is more importantly how energy saving.At present, the most public building in China and individual
The all widely used large-area glass window of house and glass curtain wall, and traditional architecture thing glass heat-proof effect is poor, this will necessarily be increased
Air conditioning electricity consumption.In order to save the energy, so people have invented following several energy-saving glass technologies, wherein mainly including hollow
Glass, coated glass, heat-reflecting glass, heat-reflecting glass film etc., these glass are provided to unnecessary in barrier sunlight
Heat radiation, so as to reach the effect of room temperature lowering.And energy-saving glass currently on the market is with pad pasting heat-protecting glass and hollow glass
Glass is relatively representative, and wherein hollow glass often occurs using divided glass as a system again, but these products
Some heat insulation are undesirable, and it is relatively low to have plenty of visible light transmissivity, have plenty of because expensive, are not easy to promote the use of, institute
To be constantly present some problems.The heat-protecting glass of showering nano-film coating is a kind of new glass heat-insulating coating, this Performances of Novel Nano-Porous
Rice glass heat-insulating coating has the advantages of visible light transmissivity is very high, and shading coefficient is relatively low, and heat insulation is relatively good, particularly
There is extraordinary transmitance to the visible ray of the 380-780 nm wave bands among sunlight, substantially can be between 50%-80%
Carry out, have good barrier simultaneously for the infrared ray of the namely 780 nm band above of the infrared band in solar radiation
Effect.At present, this nanometer heat isolation paint is the hot spot in building glass energy-saving application, after glass heat-insulating coating is made,
Coating is coated on above glass in natural conditions or the condition of extraneous drying by the mode that brushing either showering is usually used
Under cured, so as to reach very smooth, beautiful, firm film effect.Therefore, for making the thermal insulating filling in coating
Processing and develop just into the important material in glass heat-insulating coating.
The content of the invention
The defects of the object of the invention is exactly to make up prior art, there is provided a kind of doping for glass heat-insulating coating changes
The preparation method of property stannic oxide.
The present invention is achieved by the following technical solutions：
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating, including step in detail below：
（1）Appropriate citric acid is added in deionized water, adjusting pH is 1-2, is put into blender with certain speed while stirring
It is heated to 50-55 DEG C and keeps constant temperature, then adds stannic chloride pentahydrate and stir to being completely dissolved, add appropriate water sulphur afterwards
Sour manganese, ammonium fluoride, alkali source is slowly added to after at the uniform velocity stirring 10-15 minutes, is added after continuing stirring 30-340 minutes appropriate scattered
Agent, mixed liquor is obtained after stirring evenly；
（2）Mixed liquor is put into water heating kettle, 200-220 DEG C is heated to and carries out hydro-thermal reaction 120-150 minutes, after stopping reaction
Be cooled to room temperature, filter, filter cake is washed 2-3 times respectively with deionized water, absolute ethyl alcohol, then by filter cake be put into baking oven with
When 110-120 DEG C of baking 9-10 is small, be put into Muffle furnace with 600-650 DEG C carry out high-temperature calcination 2-3 it is small when, through nanometer after cooling
Pulverizer carries out attrition grinding, obtains fluorine additive Mn and is modified stannic oxide；
（3）Added after nanometer lanthanum hexaboride is mixed with the absolute ethyl alcohol that 4-5 times is measured in the reactor equipped with zirconium oxide bead, room temperature
Under ground 30-40 minutes with 1000-1200 revs/min of speed after add appropriate polyvinylpyrrolidone, be heated to 30-35 DEG C,
Discharging is into ultrasonator after when the speed grinding 5-6 of speed-raising to 2200-2400 revs/min is small, with the ultrasonic work(of 400-500W
Rate ultrasound 15-20 minutes, obtains a nanometer lanthanum hexaboride slurry；
（4）By step（2）Obtained fluorine additive Mn is modified stannic oxide and is proportionally added in nanometer lanthanum hexaboride slurry, stirs
Spray drying after mixing uniformly, you can.
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating, step（1）Described
Rotating speed with 600-800 revs/min is referred to certain speed.
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating, step（1）Described
Stannic chloride pentahydrate, manganese sulfate monohydrate, ammonium fluoride are according to 88:5:7 ratio addition.
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating, step（1）Described
Alkali source refers to sodium hydroxide, and additive amount is the 10% of stannic chloride pentahydrate quality；The dispersant refers to cetyl trimethyl
Ammonium bromide, and the 2-3% that additive amount is stannic chloride pentahydrate quality.
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating, step（3）Described
The quality of zirconium oxide bead is 3.8-4 times of nanometer lanthanum hexaboride and absolute ethyl alcohol total amount；The polyvinylpyrrolidone adds
Dosage is the 10% of nanometer lanthanum hexaboride quality.
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating, step（4）Described
It is 1 that fluorine additive Mn, which is modified stannic oxide and the additive amount ratio of nanometer lanthanum hexaboride slurry,:5.
It is an advantage of the invention that：The present invention is using hydro-thermal method by the manganese in manganese sulfate monohydrate, ammonium fluoride, Fluorin doped in dioxy
Change in tin, precipitated using sodium hydroxide as alkali source, obtained stannic oxide crystallinity is high, crystallinity is perfect；Addition ten
Six alkyl trimethyl ammonium bromides make obtained powder granule size uniform, dispersion effect is excellent as dispersant；Control conjunction at the same time
Suitable hydrothermal temperature and time so that the crystallinity of crystal is gradually perfect, and the stannic oxide through overdoping has superior
Photoelectric properties, to solar spectrum have well selectivity, have good permeability to visible ray, it is infrared to have very strong reflection
Property；Then under the action of polyethylene of dispersing agent pyrrolidones, grinding is nanometer with obtaining average grain diameter under supersonic synergetic effect
The lanthanum hexaboride slurry of rank, has the local surface plasma resonance of free electron, and resonance peak is inhaled up to 1000 nm
Wavelength is received between 750 to 1300 nm, therefore nanometer lanthanum hexaboride has substantially the near-infrared radiation in sunlight
Absorption and scattering；It is spray-dried after finally doping vario-property stannic oxide is compounded with nanometer lanthanum hexaboride, obtained production
Product particle is fine and smooth, can be added to as filler in macromolecule matrix, can be compatible and scattered equal well with macromolecule matrix
Even, heat insulation is excellent and stability is good.
Embodiment
A kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating, including step in detail below：
（1）Appropriate citric acid is added in 1L deionized waters, it is 2 to adjust pH, is put into blender and is stirred with 600 revs/min of speed side
Mix side to be heated to 50 DEG C and keep constant temperature, then add 88g stannic chloride pentahydrates and stir to being completely dissolved, add mono- water of 5g afterwards
Manganese sulfate, 7g ammonium fluorides, at the uniform velocity stir and are slowly added to 8.8g sodium hydroxides after ten minutes, and 1.7g is added after continuing stirring 30 minutes
Cetyl trimethylammonium bromide, mixed liquor is obtained after stirring evenly；
（2）Mixed liquor is put into water heating kettle, 200 DEG C is heated to and carries out hydro-thermal reaction 120 minutes, stops reaction postcooling to room
Temperature, filtering, filter cake is washed 2 times respectively with deionized water, absolute ethyl alcohol, then filter cake is put into baking oven with 110 DEG C of bakings 9
Hour, be put into Muffle furnace with 600 DEG C carry out high-temperature calcinations 2 it is small when, after cooling through nano grinder carry out attrition grinding, obtain
Fluorine additive Mn is modified stannic oxide；
（3）Added after 100g nanometers of lanthanum hexaborides are mixed with 400ml absolute ethyl alcohols in the reactor equipped with zirconium oxide bead, room temperature
Under ground 30 minutes with 1000 revs/min of speed after add 10g polyvinylpyrrolidones, be heated to 30 DEG C, raise speed to 2200 turns/
Discharging is 15 minutes ultrasonic with the ultrasonic power of 400W into ultrasonator after when the speed grinding 5 divided is small, obtains six boron of nanometer
Change lanthanum slurry；
（4）By step（2）Obtained fluorine additive Mn is modified stannic oxide according to 1:5 ratio is mixed with nanometer lanthanum hexaboride slurry
Uniformly, it is spray-dried after stirring evenly, you can.
Claims (6)
1. the preparation method of a kind of doping vario-property stannic oxide for glass heat-insulating coating, it is characterised in that including following tool
Body step：
（1）Appropriate citric acid is added in deionized water, adjusting pH is 1-2, is put into blender with certain speed while stirring
It is heated to 50-55 DEG C and keeps constant temperature, then adds stannic chloride pentahydrate and stir to being completely dissolved, add appropriate water sulphur afterwards
Sour manganese, ammonium fluoride, alkali source is slowly added to after at the uniform velocity stirring 10-15 minutes, is added after continuing stirring 30-340 minutes appropriate scattered
Agent, mixed liquor is obtained after stirring evenly；
（2）Mixed liquor is put into water heating kettle, 200-220 DEG C is heated to and carries out hydro-thermal reaction 120-150 minutes, after stopping reaction
Be cooled to room temperature, filter, filter cake is washed 2-3 times respectively with deionized water, absolute ethyl alcohol, then by filter cake be put into baking oven with
When 110-120 DEG C of baking 9-10 is small, be put into Muffle furnace with 600-650 DEG C carry out high-temperature calcination 2-3 it is small when, through nanometer after cooling
Pulverizer carries out attrition grinding, obtains fluorine additive Mn and is modified stannic oxide；
（3）Added after nanometer lanthanum hexaboride is mixed with the absolute ethyl alcohol that 4-5 times is measured in the reactor equipped with zirconium oxide bead, room temperature
Under ground 30-40 minutes with 1000-1200 revs/min of speed after add appropriate polyvinylpyrrolidone, be heated to 30-35 DEG C,
Discharging is into ultrasonator after when the speed grinding 5-6 of speed-raising to 2200-2400 revs/min is small, with the ultrasonic work(of 400-500W
Rate ultrasound 15-20 minutes, obtains a nanometer lanthanum hexaboride slurry；
（4）By step（2）Obtained fluorine additive Mn is modified stannic oxide and is proportionally added in nanometer lanthanum hexaboride slurry, stirs
Spray drying after mixing uniformly, you can.
2. a kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating according to claim 1, its
It is characterized in that, step（1）The rotating speed referred to certain speed with 600-800 revs/min.
3. a kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating according to claim 1, its
It is characterized in that, step（1）The stannic chloride pentahydrate, manganese sulfate monohydrate, ammonium fluoride are according to 88:5:7 ratio addition.
4. a kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating according to claim 1, its
It is characterized in that, step（1）The alkali source refers to sodium hydroxide, and additive amount is the 10% of stannic chloride pentahydrate quality；Point
Powder refers to cetyl trimethylammonium bromide, and the 2-3% that additive amount is stannic chloride pentahydrate quality.
5. a kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating according to claim 1, its
It is characterized in that, step（3）The quality of the zirconium oxide bead is 3.8-4 times of nanometer lanthanum hexaboride and absolute ethyl alcohol total amount；Institute
The additive amount for the polyvinylpyrrolidone stated is the 10% of nanometer lanthanum hexaboride quality.
6. a kind of preparation method of doping vario-property stannic oxide for glass heat-insulating coating according to claim 1, its
It is characterized in that, step（4）It is 1 that the fluorine additive Mn, which is modified stannic oxide and the additive amount ratio of nanometer lanthanum hexaboride slurry,:
5。
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0905100A1 (en) * | 1997-09-30 | 1999-03-31 | Sumitomo Metal Mining Company Limited | Coating solution for forming a selectively transmitting film |
-
2017
- 2017-10-30 CN CN201711033188.XA patent/CN107974105A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0905100A1 (en) * | 1997-09-30 | 1999-03-31 | Sumitomo Metal Mining Company Limited | Coating solution for forming a selectively transmitting film |
Non-Patent Citations (2)
| Title |
|---|
| 吴志军: "F_Mn共掺杂SnO_2改性水性聚氨酯的制备及性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 阮文科: "LaB_6纳米隔热浆料的制备及其在隔热透明涂料的应用研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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