CN106243664A - Ferrum/nitrogen-doped titanic acid lanthanio infrared composite material and preparation method thereof - Google Patents
Ferrum/nitrogen-doped titanic acid lanthanio infrared composite material and preparation method thereof Download PDFInfo
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- CN106243664A CN106243664A CN201610757296.0A CN201610757296A CN106243664A CN 106243664 A CN106243664 A CN 106243664A CN 201610757296 A CN201610757296 A CN 201610757296A CN 106243664 A CN106243664 A CN 106243664A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/08—Polyesters modified with higher fatty oils or their acids, or with resins or resin acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
Open a kind of ferrum/nitrogen-doped titanic acid lanthanio infrared composite material of the present invention and preparation method thereof.The composition of infrared composite material and weight percentage be: filmogen, 57～67, brick-red infrared filler, 24～29, solvent, 8～13, defoamer, 0.5, and thickening agent, 0.5；Wherein, described brick-red infrared filler formula is La1‑ xFexTi(O,N)3Powder, in formula, x=0.0,0.1,0.3,0.5,0.7 or 1.0.Preparation method includes: by the raw material mixing of brick-red infrared filler, heating in water bath, pretreatment, be dried, calcining, ammonolysis, obtain brick-red powder；And press infrared composite material proportioning first by filmogen, solvent, defoamer and thickening agent mixing and stirring, add brick-red infrared filling material grinding and uniformly make it fully dispersed, obtain infrared composite material.The composite of the present invention, environmental friendliness, heat-proof quality is good.
Description
Technical field
The invention belongs to infrared composite material technical field, particularly a kind of environmental friendliness, cheap, heat-proof quality good
Ferrum/nitrogen-doped titanic acid lanthanio infrared composite material and preparation method thereof.
Background technology
The 98% of solar radiation energy (includes ultraviolet, visible light wave range and near-infrared ripple in being at 0.15～3 mu m wavebands
Section), wherein to account for the sun total for visible light wave range (400nm-700nm) and near infrared band (700-2500nm) total radiation energy sum
About the 95% of emittance.The object under shining upon just can be made to become if able to visible ray and near infrared light are reflected
Nice and cool, to save the energy.
At present, the material with reflecting properties has been carried out a lot of research by domestic and international researcher and mechanism, especially
It is the reflecting properties research near infrared band.True field and person of outstanding talent have studied the application in practice of infrared reflection performance, and it is adopted
The near-infrared reflection performance of black pigment, coating and resin combination can reach about 65% (true field and person of outstanding talent, infrared ray
Reflection black pigment, coating and resin combination, State Intellectual Property Office of the People's Republic of China, 2008).Martin-raise
Lignum Rhamnellae have studied the oxide-nitride base coloring pigment of three kinds of crystal structures, has widened the chromatographic breadth of coloring pigment and has increased
Strong color intensity (CN95108649-oxide-nitride base coloring pigment and preparation thereof and purposes .1995).Much grind
Study carefully mechanism and find preparation technology and the optimal conditions of infrared composite material nontoxic, high performance, to replace tradition the most urgently
Poisonous low performance material, thus adapt to society to environmental conservation and the requirement of properties of product.
But, above-mentioned reflecting material preparation method generally exist preparation temperature height, response time length, raw material sources difficulty,
Apply the problems such as the most extensive.Meanwhile, during as infrared composite material, its heat-proof quality is not furtherd investigate.
In a word, present technology there is the problem that infrared reflective material heat-proof quality is bad, environment is unfriendly, and cost is high.
Summary of the invention
It is an object of the invention to provide a kind of ferrum/nitrogen-doped titanic acid lanthanio infrared composite material, heat-proof quality is good, environment
Close friend, with low cost.
Another object of the present invention is to provide the preparation method of a kind of ferrum/nitrogen-doped titanic acid lanthanio infrared composite material.
The technical solution realizing the object of the invention is:
A kind of ferrum/nitrogen-doped titanic acid lanthanio infrared composite material, it forms and weight percentage is:
Filmogen, 57～67；
Brick-red infrared filler, 24～29；
Solvent, 8～13；
Defoamer, 0.5；
Thickening agent, 0.5；
Wherein, described brick-red infrared filler is La1-xFexTi(O,N)3Powder, in formula, x=0,0.1,0.3,0.5,0.7,
1.0。
Preferably, described filmogen is alkyd varnish.
Preferably, described solvent is rosin.
Preferably, described defoamer is DC-65 organic silicon defoamer.
Preferably, described thickening agent is sodium carboxymethyl cellulose.
The technical solution realizing another object of the present invention is:
A kind of ferrum/nitrogen-doped titanic acid lanthanio infrared composite material and preparation method thereof, comprises the steps:
(10) brick-red infrared filler is prepared: by the raw material mixing of brick-red infrared filler, heating in water bath, pretreatment, be dried, forge
Burning, ammonolysis, obtain brick-red infrared filler powder, stand-by；
(20) batch mixing: by proportioning first by filmogen, solvent, defoamer and thickening agent mixing and stirring, add brick-red
Infrared filling material grinding uniformly makes it fully dispersed, obtains infrared composite material.
Preferably, described (10) prepare brick-red infrared filler step and include:
(11) raw material mixing: butyl titanate is dissolved in ethylene glycol, obtains milky thickness base fluid, by lanthanum nitrate hexahydrate and
Fe(NO3)39H2O is stirred at room temperature and is dissolved in above-mentioned thickness base fluid, obtains reactant liquor；
(12) heating in water bath: by described reactant liquor heating in water bath, stirring is slowly added monohydrate potassium；
(13) pretreatment: continue stirring, using ammonia spirit as neutralization reagent and reaction promoter, regulates reactant liquor pH value, and
Continue to heat up, obtain viscous liquid；
(14) it is dried: above-mentioned viscous liquid is put in baking oven and be dried, obtain xerogel；
(15) calcining: put into after being ground by xerogel in Muffle furnace and calcine, prepares precursor powder；
(16) ammonolysis: above-mentioned precursor powder is placed in tube furnace, ammonolysis, furnace cooling under ammonia atmosphere, grinds, obtains
Described brick-red infrared filler powder.
Preferably, in the mixing of described (11) raw material and (12) heating in water bath step, Fe(NO3)39H2O, six nitric hydrates
Lanthanum, butyl titanate, the weight ratio of monohydrate potassium are (0～24.24): (19.50～0): 20.42:75.65.
Preferably, in described (12) heating in water bath step, heating-up temperature is 85 DEG C, and heat time heating time is 3h.
Preferably, in described (13) pre-treatment step, ammonia spirit concentration is 1～4mol/L, reactant liquor PH regulation to 8～
9。
Preferably, in described (14) drying steps, baking temperature is 100～130 DEG C, and drying time is 4～10h.
Preferably, in described (15) calcining step, calcining heat is 700～950 DEG C, and calcination time is 2～4h.
Preferably, in described (16) aminolysis step, ammonolysis temperature is 800～1000 DEG C, and the ammonolysis time is 3～5h.
Compared with prior art, its remarkable advantage is the present invention:
1, heat-proof quality is good: the La of preparation1-xFexTi(O,N)3Powder, due to intratomic or interatomic charge transtion, in brick
Red and near infrared band, there is good reflecting properties, can effectively reflect near infrared band emittance, therefore this patent
Infrared composite material, compared with the infrared composite material of existing Similar color, have and preferably intercept solar thermal energy to painting
The performance of layer internal delivery, it is possible to decrease indoor temperature 4.2 DEG C～4.5 DEG C；
2, environmental friendliness: without heavy metallic oxides such as Pb, Cd, Cr, Ni, beneficially environmental conservation and human health；
3, low cost: preparation method is simple, and synthesis device and raw material are easy to get, with low cost.
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is heat-proof quality experimental apparatus for testing figure.
Detailed description of the invention
For ease of it is further understood that the present invention, following example are all by identical preparation method system
Standby.
First, brick-red infrared filler is prepared: by the raw material mixing of brick-red infrared filler, heating in water bath, pretreatment, do
Dry, calcining, ammonolysis, obtain brick-red infrared filler powder；Wherein, raw material lanthanum nitrate hexahydrate, Fe(NO3)39H2O, metatitanic acid four
Butyl ester, monohydrate potassium are commercially available analytical pure.Brick-red infrared filler material proportioning is as shown in table 1, thus obtains formula
For La1-xFexTi(O,N)3Powder, as shown in table 1.
The brick-red infrared filler material proportioning of table 1 and brick-red infrared filler component list
Then, batch mixing: filmogen, solvent, defoamer and thickening agent are first mixed by the infrared composite material proportioning as shown in table 2
Stir, add brick-red infrared filling material grinding and uniformly make it fully dispersed, obtain infrared composite material.
Wherein, alkyd varnish, rosin, DC-65 organic silicon defoamer and sodium carboxymethyl cellulose are marketable material.
Table 2 infrared composite material proportioning table
The infrared composite material of embodiment and comparative example is uniformly painted on iron plate (thickness 2mm) by standard JG/T 23-2001
On, brush thickness is 60 μm, places 7 days, make infrared composite material test board after brushing under natural environment.
For checking the effect of heat insulation of ferrum of the present invention/nitrogen-doped titanic acid lanthanio infrared composite material, by embodiment described in table 2
Infrared composite material with by commercially available ferric oxide red colorant by the method for mixing identical with the infrared composite material in embodiment
The material (comparative example) prepared compares.The device that comparative experiments uses is as shown in Figure 1.Wherein test instrunment includes: near-infrared
Lamp (BR 125 IR Red, 250 W)；Digital thermometer (VC6801A).
Unit simulation tilting building and make, wherein, casing is hollow, four sides and base material be polystyrene foam plate,
Thickness is 10mm, the length × width × height of casingmax× highminIt is 80 × 80 × 150 × 120mm, solid in the one side perforate of casing
Fixed temperature meter is popped one's head in, and probe is positioned at casing center, specifically comprises the following steps that
(1) the infrared composite material test board will prepared by embodiment and comparative example, is placed on above casing, the one side of brushing paint
Upward, the geometric center of two tanks should be immediately below the center of bulb, and two tanks adjacent surface is at a distance of 40mm；
(2) distance between near-infrared lamp and casing peak is 150mm, opens regulated power supply, 20 minutes latter two casings
Inside Air Temperature is stable, and thermometer display numerical value is basically unchanged.Calculating temperature gap in two tanks, result is as shown in table 3.Temperature
Spend the internal temperature of the internal temperature comparative example casing of poor=embodiment casing.
Box interior temperature between table 3 embodiment and comparative example is poor
| Embodiment | 1 | 2 | 3 | 4 | 5 | 6 |
| Temperature difference (DEG C) | -4.3 | -4.2 | -4.5 | -4.4 | -4.5 | -4.2 |
Test result from table 3, it can be seen that box interior temperature corresponding to various embodiments of the present invention, is below comparative example
Corresponding box interior temperature, difference is respectively-4.3 DEG C ,-4.2 DEG C ,-4.5 DEG C ,-4.4 DEG C ,-4.5 DEG C ,-4.2 DEG C.The present invention
Ferrum/nitrogen-doped titanic acid lanthanio infrared composite material can effectively intercept solar thermal energy to coat inside transmit, reduce inside
Space temperature, saves hot weather energy consumption for cooling, alleviates the effect of urban heat land effect.And, raw material and finished product all do not contain
The heavy metallic oxides such as Cd, Cr, Ni, beneficially environmental conservation and human health；Preparation method is simple, and synthesis device and raw material are easy
, with low cost.
Claims (13)
1. ferrum/nitrogen-doped titanic acid lanthanio infrared composite material, it forms and weight percentage is:
Filmogen, 57～67；
Brick-red infrared filler, 24～29；
Solvent, 8～13；
Defoamer, 0.5
Thickening agent, 0.5；
Wherein, described brick-red infrared filler is La1-xFexTi(O,N)3Powder, in formula, x=0.0,0.1,0.3,0.5,0.7 or
1.0。
Infrared composite material the most according to claim 1, it is characterised in that: described filmogen is alkyd varnish.
Infrared composite material the most according to claim 1, it is characterised in that: described solvent is rosin.
Infrared composite material the most according to claim 1, it is characterised in that: described defoamer is DC-65 organosilicon froth breaking
Agent.
Infrared composite material the most according to claim 1, it is characterised in that: described thickening agent is sodium carboxymethyl cellulose.
6. a preparation method for ferrum as claimed in claim 1/nitrogen-doped titanic acid lanthanio infrared composite material, including walking as follows
Rapid:
(10) brick-red infrared filler is prepared: by the raw material mixing of brick-red infrared filler, heating in water bath, pretreatment, be dried, forge
Burning, ammonolysis, obtain brick-red infrared filler powder, stand-by；
(20) batch mixing: by proportioning first by filmogen, solvent, defoamer and thickening agent mixing and stirring, add brick-red
Infrared filling material grinding uniformly makes it fully dispersed, obtains infrared composite material.
Preparation method the most according to claim 6, it is characterised in that: described prepare brick-red infrared filler step and include:
(11) raw material mixing: butyl titanate is dissolved in ethylene glycol, obtains milky thickness base fluid, by lanthanum nitrate hexahydrate and
Fe(NO3)39H2O is stirred at room temperature and is dissolved in above-mentioned thickness base fluid, obtains reactant liquor；
(12) heating in water bath: by described reactant liquor heating in water bath, stirring is slowly added monohydrate potassium；
(13) pretreatment: continue to stir using ammonia spirit as neutralization reagent and reaction promoter, regulate reactant liquor pH value, and continue
Temperature of continuing rising, obtains viscous liquid；
(14) being dried: by above-mentioned, viscous liquid is put in baking oven and is dried, and obtains xerogel；
(15) calcining: put into after being ground by xerogel in Muffle furnace and calcine, prepares precursor powder；
(16) ammonolysis: above-mentioned precursor powder is placed in tube furnace, ammonolysis, furnace cooling under ammonia atmosphere, grinds, obtains
Described brick-red infrared filler powder.
Red preparation method the most according to claim 7, it is characterised in that: the mixing of described (11) raw material and (12) heating in water bath
In step, Fe(NO3)39H2O, lanthanum nitrate hexahydrate, butyl titanate, the weight ratio of monohydrate potassium are (0～24.24):
(19.50～0): 20.42:75.65.
Infrared composite material preparation method the most according to claim 7, it is characterised in that: described (12) heating in water bath step
In, heating-up temperature is 85 DEG C, and heat time heating time is 3h.
Preparation method the most according to claim 7, it is characterised in that: in described (13) pre-treatment step, ammonia spirit is dense
Degree is 1～4mol/L, and reactant liquor PH regulates to 8～9.
11. preparation methoies according to claim 7, it is characterised in that: in described (14) drying steps, baking temperature is
100～130 DEG C, drying time is 4～10h.
12. preparation method for material according to claim 7, it is characterised in that: in described (15) calcining step, calcining heat is
700～950 DEG C, calcination time is 2～4h.
13. preparation methoies according to claim 7, it is characterised in that: in described (16) aminolysis step, ammonolysis temperature is
800～1000 DEG C, the ammonolysis time is 3～5h.
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| CN201610757296.0A CN106243664B (en) | 2016-08-27 | 2016-08-27 | Iron/nitrogen-doped titanic acid lanthanum base infrared composite material and preparation method thereof |
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|---|---|---|---|
| CN201610757296.0A CN106243664B (en) | 2016-08-27 | 2016-08-27 | Iron/nitrogen-doped titanic acid lanthanum base infrared composite material and preparation method thereof |
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| CN106243664B CN106243664B (en) | 2017-12-12 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040024071A1 (en) * | 2002-08-01 | 2004-02-05 | Meier Paul F. | Perovskite compositions and method of making and process of using such compositions |
| JP2004221239A (en) * | 2003-01-14 | 2004-08-05 | Matsushita Electric Ind Co Ltd | Thin film formation method |
| CN101298367A (en) * | 2008-03-04 | 2008-11-05 | 中国计量学院 | Preparation of BLT composite glass phase ferroelectric film |
| CN101899249A (en) * | 2009-05-25 | 2010-12-01 | 上海复甲新型材料科技有限公司 | Transparent thermal insulation anti-ultraviolet coating and preparation method thereof |
| CN104355617A (en) * | 2014-10-27 | 2015-02-18 | 吉林大学 | High-temperature and high-pressure preparation method of cubic phase lanthanum, iron and titanium oxide |
-
2016
- 2016-08-27 CN CN201610757296.0A patent/CN106243664B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040024071A1 (en) * | 2002-08-01 | 2004-02-05 | Meier Paul F. | Perovskite compositions and method of making and process of using such compositions |
| JP2004221239A (en) * | 2003-01-14 | 2004-08-05 | Matsushita Electric Ind Co Ltd | Thin film formation method |
| CN101298367A (en) * | 2008-03-04 | 2008-11-05 | 中国计量学院 | Preparation of BLT composite glass phase ferroelectric film |
| CN101899249A (en) * | 2009-05-25 | 2010-12-01 | 上海复甲新型材料科技有限公司 | Transparent thermal insulation anti-ultraviolet coating and preparation method thereof |
| CN104355617A (en) * | 2014-10-27 | 2015-02-18 | 吉林大学 | High-temperature and high-pressure preparation method of cubic phase lanthanum, iron and titanium oxide |
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