CN106318162B - Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof - Google Patents
Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof Download PDFInfo
- Publication number
- CN106318162B CN106318162B CN201610739948.8A CN201610739948A CN106318162B CN 106318162 B CN106318162 B CN 106318162B CN 201610739948 A CN201610739948 A CN 201610739948A CN 106318162 B CN106318162 B CN 106318162B
- Authority
- CN
- China
- Prior art keywords
- infrared
- brown
- composite material
- filler
- ammonolysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
- C09D167/08—Polyesters modified with higher fatty oils or their acids, or with natural resins or resin acids
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/004—Reflecting paints; Signal paints
Abstract
The present invention discloses iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof, and the composition and weight percentage of infrared composite material of the invention are filmogen: 67-61, the infrared filler of brown: 24-27, solvent: 8-11, defoaming agent: 0.5, thickener: 0.5；Wherein, the infrared filler general formula of the brown is Mg1‑xFexTi(O,N)3Powder, in formula, x=0.0,0.1,0.2 or 0.3.Preparation method of the invention includes: that raw material mixing, heating water bath, solation, drying, the calcining, ammonolysis of the infrared filler of brown are obtained the infrared filler powder of brown；And first filmogen, solvent, defoaming agent and thickener are mixed evenly by infrared composite material proportion, adding the infrared filling material grinding of brown uniformly makes its fully dispersed, obtains infrared composite material.Composite material of the invention, environmental-friendly, heat-proof quality is good.
Description
Technical field
The invention belongs to infrared composite material technical field, especially it is a kind of it is environmental-friendly, cheap, barrier property is good
Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof.
Background technique
The 98% of solar radiation energy is in 0.15~3 mu m waveband (including ultraviolet, visible light wave range and near-infrared wave
Section), wherein visible light wave range (400nm-700nm) and near infrared band (700-2500nm) totally account for total solar radiation amount
95% or so, so if can be effectively it will be seen that the object under light and near infrared light reflection can make to shine upon becomes
Nice and cool, this, which is not only saved energy, also provides new thinking for the development that continues of infrared composite material.
Currently, researcher and mechanism have carried out many researchs to the material with reflecting properties both at home and abroad, especially
It is the reflecting properties research near infrared band.True field and person of outstanding talent have studied the application of infrared reflection performance in practice, adopt
The near-infrared reflection performance of black pigment, coating and resin combination can achieve 65% or so (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-raises
The oxide-nitride base coloring pigment for having studied three kinds of crystal structures such as gloomy, has widened the chromatographic breadth of coloring pigment and increasing
Strong color intensity (CN95108649- oxide-nitride base coloring pigment and its preparation and use .1995).Much grind
Mechanism is studied carefully also urgently in the preparation process and optimal conditions for finding nontoxic, high performance infrared composite material, to replace tradition
Toxic low performance material, to adapt to requirement of the society to environmental protection and properties of product.
However, since there are preparation temperature height, the reaction time is long, raw material sources are difficult, using wideless in above-mentioned method
The problems such as general, when especially as a kind of infrared composite material, not deeper into research its heat-proof quality, therefore the present invention mentions
A kind of out preparation method is simple, and raw material sources are extensive, cheap, and physicochemical properties are stable and heat-proof quality is good one
Kind material.
Summary of the invention
The purpose of the present invention is to provide iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof, composite woods
Material is free of poisonous and harmful heavy metallic oxide, and environmental-friendly, heat-proof quality is good.
The technical solution for realizing the aim of the invention is as follows: iron/nitrogen-doped titanic acid magnesium-based infrared composite material, composition and
Weight percentage is filmogen: 57-67, the infrared filler of brown: 24-29, solvent: 8-13, defoaming agent: 0.5, thickener:
0.5；Wherein, the infrared filler general formula of the brown is Mg1-xFexTi(O,N)3Powder, in formula, x=0.0,0.1,0.2,0.3.
Preferably, the filmogen is alkyd varnish.
Preferably, the solvent is rosin.
Preferably, the defoaming agent is DC-65 organic silicon defoamer.
Preferably, the thickener is sodium carboxymethylcellulose.
Realize the technical solution of another object of the present invention are as follows: iron/nitrogen-doped titanic acid magnesium-based infrared composite material and its
Preparation method includes the following steps:
10) it prepares the infrared filler of brown: by the raw material mixing of the infrared filler of brown, heating water bath, pretreatment, drying, forging
It burns, ammonolysis, obtains the infrared filler powder of brown；
20) mixing: first filmogen, solvent, defoaming agent and thickener are mixed by the proportion of infrared composite material shown in table 2
Conjunction stirs evenly, and adding the infrared filling material grinding of brown uniformly makes its fully dispersed, obtains infrared composite material.
Preferably, the infrared filler step of preparation brown includes:
11) raw material mixes: by a certain amount of magnesium nitrate hexahydrate, Fe(NO3)39H2O, monohydrate potassium and acryloyl
Amine is dissolved in deionized water according to a certain percentage, obtains transparent mixed solution after mixing uniformly；
12) heating water bath: the reaction solution heating water bath is stirred to after being completely dissolved, and continues stirring a period of time；
13) solation: in the process, the isopropanol organic liquor containing a certain amount of butyl titanate is added drop-wise to mixing above
In solution, heats and stir, obtain colloidal sol；
14) dry: viscous liquid obtained above being placed in oven and dried, xerogel is obtained；
15) it calcines: being put into Muffle furnace and calcine after xerogel is ground, precursor powder is made；
16) ammonolysis: above-mentioned precursor powder being placed in tube furnace, ammonolysis, furnace cooling (under ammonia atmosphere), grinding,
Obtain the infrared filler powder Mg of the brown1-xFexTi(O,N)3, wherein x=0.0,0.1,0.2,0.3.
Preferably, in described raw material mixing (11) step, Fe(NO3)39H2O, magnesium nitrate hexahydrate, butyl titanate, one
The weight ratio of citric acid monohydrate and acrylamide is (0.00-7.27): (15.38-10.77): 20.42:75.65:34.12.
Preferably, in heating water bath (12) step, heating temperature is 85 DEG C, heating time 3h.
Preferably, in solation (13) step, heating temperature is 85 DEG C, heating time 2h.
Preferably, in drying (14) step, drying temperature is 100~130 DEG C, and drying time is 4~10h.
Preferably, in described calcining (15) step, calcination temperature is 700-950 DEG C, calcination time 2-4h.
Preferably, in ammonolysis (16) step, ammonolysis temperature is 800~1000 DEG C, and the ammonolysis time is 3~5h.
Compared with prior art, the present invention its remarkable advantage:
1, heat-proof quality is good: the Mg of preparation1-xFexTi(O,N)3Powder is in due to intratomic or interatomic charge transtion
Brown and near infrared band have good reflecting properties, can effectively reflect near infrared band radiation energy, therefore this patent
Infrared composite material, compared with the infrared composite material of existing Similar color, have preferably barrier solar thermal energy to painting
The internal performance transmitted of layer, can reduce by 6.2 DEG C -7.4 DEG C of room temperature；
2, environmental-friendly: without heavy metallic oxides such as Pb, Cd, Cr, Ni, to be conducive to environmental protection and human health；
3, at low cost: preparation method is simple, and synthesis device and raw material are easy to get, low in cost.
The present invention is described in further detail With reference to embodiment.
Detailed description of the invention
Fig. 1 is the infrared filler material of brown with the when infrared filler component list of brown.
Fig. 2 is that infrared composite material matches table.
Fig. 3 is heat-proof quality experimental apparatus for testing figure.
Box interior temperature difference table of the Fig. 4 between embodiment and comparative example.
Specific embodiment
For convenient for it is further understood that the present invention, following embodiment press identical preparation method system
It is standby.
Firstly, preparation the infrared filler of brown: by the raw material mixing of the infrared filler of brown, heating water bath, pretreatment, drying,
Calcining, ammonolysis, obtain the infrared filler powder of brown；Wherein, raw material magnesium nitrate hexahydrate, Fe(NO3)39H2O, butyl titanate,
Monohydrate potassium and acrylamide are that commercially available analysis is pure.The infrared filler material proportion of brown is as shown in table 1, to be led to
Formula is Mg1-xFexTi(O,N)3Powder, as shown in table 1.
Then, mixing: by the proportion of infrared composite material shown in table 2 first by filmogen, solvent, defoaming agent and thickener
It is mixed evenly, adding the infrared filling material grinding of brown uniformly makes its fully dispersed, obtains infrared composite material.
Wherein, alkyd varnish, rosin, DC-65 organic silicon defoamer and sodium carboxymethylcellulose are marketable material.
The infrared composite material of embodiment and comparative example is uniformly painted on aluminium sheet (thickness by standard JG/T 23-2001
On 2mm), brush is placed 7 days in a natural environment with a thickness of 60 μm after brushing, and infrared composite material test board is made.
It, will be in embodiment described in table 2 for the heat insulation for examining iron/nitrogen-doped titanic acid magnesium-based infrared composite material of the present invention
Infrared composite material with by commercially available ferric oxide red colorant press method for mixing identical with the infrared composite material in embodiment
Material (comparative example) obtained compares.The device that comparative experiments uses is as shown in Figure 3.Wherein test equipment includes: near-infrared
Lamp (BR 125IR Red, 250W)；Digital thermometer (VC6801A).
Unit simulation tilting building and make, wherein cabinet be it is hollow, four sides and base material be polystyrene foam plate,
With a thickness of 10mm, length × width × height max × high min of cabinet is 80 × 80 × 150 × 120mm, solid in the one side aperture of cabinet
Determine thermometer probe, probe is located at cabinet center, the specific steps are as follows:
(1) it by by the infrared composite material test board of embodiment and comparative example preparation, is placed on above cabinet, brushing paint
On one side upward, the geometric center of two tanks should be immediately below the center of light bulb, and two tanks adjacent surface is at a distance of 40mm；
(2) the distance between near-infrared lamp and cabinet highest point are 150mm, open regulated power supply, after twenty minutes two casees
The Inside Air Temperature of body is stablized, and thermometer shows that numerical value is basically unchanged.Temperature gap in two tanks is calculated, as a result such as 3 institute of table
Show.Temperature difference=embodiment cabinet internal temperature-comparative example cabinet internal temperature.
It can be seen that the corresponding box interior temperature of various embodiments of the present invention from the test result in table 3, be below pair
The corresponding box interior temperature of ratio, difference are respectively -6.9 DEG C, -6.2 DEG C, -7.0 DEG C, -6.3 DEG C, -7.4 DEG C, -7.1 DEG C.This
The iron of invention/nitrogen-doped titanic acid magnesium-based infrared composite material can effectively obstruct solar thermal energy and transmit to coat inside, reach reduction
Interior space temperature saves hot weather energy consumption for cooling, alleviates the effect of urban heat land effect.Moreover, in raw material and finished product
Without heavy metallic oxides such as Cd, Cr, Ni, be conducive to environmental protection and human health；Preparation method is simple, synthesis device and original
Material is easy to get, low in cost.
Claims (2)
1. a kind of iron/nitrogen-doped titanic acid magnesium-based infrared composite material, composition and weight percentage are,
Filmogen: 67-61；
The infrared filler of brown: 24-27；
Solvent: 8-11；
Defoaming agent: 0.5；
Thickener: 0.5；
Wherein, the infrared filler of the brown is Mg1-xFexTi(O,N)3Powder, in formula, x=0.1,0.2,0.3；
The defoaming agent is DC-65 organic silicon defoamer；
The thickener is sodium carboxymethylcellulose.
2. a kind of iron as described in claim 1/nitrogen-doped titanic acid magnesium-based infrared composite material preparation method, including walk as follows
It is rapid:
(10) prepare the infrared filler of brown: by the raw material mixing of the infrared filler of brown, heating water bath, solation, drying, calcining,
Ammonolysis obtains the infrared filler powder of brown；
(20) mixing: first filmogen, solvent, defoaming agent and thickener being mixed evenly by infrared composite material proportion,
Adding the infrared filling material grinding of brown uniformly makes its fully dispersed, obtains infrared composite material；
Described (10) prepare the infrared filler step of brown
(11) raw material mixes: a certain amount of magnesium nitrate hexahydrate, Fe(NO3)39H2O, monohydrate potassium and acrylamide are pressed
Certain ratio is dissolved in deionized water, obtains transparent mixed solution after mixing uniformly；
(12) it heating water bath: by the reaction solution heating water bath and stirs to after dissolving, continues stirring a period of time；
(13) solation: in the process, it is molten that the isopropanol organic liquor containing a certain amount of butyl titanate is added drop-wise to mixing above
In liquid, heats and stir, obtain colloidal sol；
(14) dry: viscous liquid obtained above being placed in oven and dried, xerogel is obtained；
(15) it calcines: being put into Muffle furnace and calcine after xerogel is ground, precursor powder is made；
(16) ammonolysis: above-mentioned precursor powder being placed in tube furnace, ammonolysis, the furnace cooling under ammonia atmosphere, and grinding obtains
The infrared filler powder Mg of brown1-xFexTi(O,N)3, wherein x=0.1,0.2,0.3；
In (11) the raw material mixing step, Fe(NO3)39H2O, magnesium nitrate hexahydrate, monohydrate potassium and acrylamide
Weight ratio is 2.42:13.85:75.65:34.12 or 4.84:12.31:75.65:34.12 or 7.27:10.77:75.65:
34.12；
In (12) the heating water bath step, heating temperature is 85 DEG C, heating time 3h；
In (13) the solation step, heating temperature is 85 DEG C, heating time 2h；
In (14) drying steps, drying temperature is 100~130 DEG C, and drying time is 4~10h；
In (15) calcining step, calcination temperature is 700-950 DEG C, calcination time 2-4h；
In (16) aminolysis step, ammonolysis temperature is 800~1000 DEG C, and the ammonolysis time is 3~5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610739948.8A CN106318162B (en) | 2016-08-27 | 2016-08-27 | Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610739948.8A CN106318162B (en) | 2016-08-27 | 2016-08-27 | Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106318162A CN106318162A (en) | 2017-01-11 |
| CN106318162B true CN106318162B (en) | 2019-06-21 |
Family
ID=57790949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610739948.8A Expired - Fee Related CN106318162B (en) | 2016-08-27 | 2016-08-27 | Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106318162B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109467745A (en) * | 2018-12-14 | 2019-03-15 | 江南大学 | A kind of near-infrared reflection raw powder's production technology |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121944A (en) * | 1994-08-19 | 1996-05-08 | 凯尔迪克陶瓷颜料股份公司 | Coloured pigments based on oxide-nitrides, the preparation and use thereof |
| EP1020509A1 (en) * | 1999-01-16 | 2000-07-19 | Philips Patentverwaltung GmbH | Colour display panel with colour pigment |
| CN1376634A (en) * | 2002-04-22 | 2002-10-30 | 中国科学院上海硅酸盐研究所 | Process for preparing nano titanium chromium nitride oxide powder |
| CN101058680A (en) * | 2006-04-21 | 2007-10-24 | 默克专利股份有限公司 | Pigment |
| CN104119720A (en) * | 2014-06-07 | 2014-10-29 | 内蒙古大学 | Red pigment capable of reflecting near infrared radiation |
| CN104250514A (en) * | 2014-09-25 | 2014-12-31 | 南京理工大学 | Deep brown near-infrared reflection type heat insulation coating and preparation method thereof |
| CN104830139A (en) * | 2015-05-12 | 2015-08-12 | 南京理工大学 | Green porous near-infrared reflection pigment and preparation method thereof |
-
2016
- 2016-08-27 CN CN201610739948.8A patent/CN106318162B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1121944A (en) * | 1994-08-19 | 1996-05-08 | 凯尔迪克陶瓷颜料股份公司 | Coloured pigments based on oxide-nitrides, the preparation and use thereof |
| EP1020509A1 (en) * | 1999-01-16 | 2000-07-19 | Philips Patentverwaltung GmbH | Colour display panel with colour pigment |
| CN1376634A (en) * | 2002-04-22 | 2002-10-30 | 中国科学院上海硅酸盐研究所 | Process for preparing nano titanium chromium nitride oxide powder |
| CN101058680A (en) * | 2006-04-21 | 2007-10-24 | 默克专利股份有限公司 | Pigment |
| CN104119720A (en) * | 2014-06-07 | 2014-10-29 | 内蒙古大学 | Red pigment capable of reflecting near infrared radiation |
| CN104250514A (en) * | 2014-09-25 | 2014-12-31 | 南京理工大学 | Deep brown near-infrared reflection type heat insulation coating and preparation method thereof |
| CN104830139A (en) * | 2015-05-12 | 2015-08-12 | 南京理工大学 | Green porous near-infrared reflection pigment and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Synthesis and characterization of Al3+ doped LaFeO3 compounds:A novel inorganic pigments with high near-infrared reflectance;Lili Liu et al.;《Solar Energy Materials & Solar Cells》;20141007;第132卷;第377–384页 |
| Synthesis and characterization of blue TiO2/CoAl2O4 complex pigments with good colour and enhanced near-infrared reflectance properties;Wei Zheng et al.;《The Royal Society of Chemistry》;20151012;第5卷;第87932-87939页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106318162A (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Han et al. | Estimating thermal performance of cool coatings colored with high near-infrared reflective inorganic pigments: Iron doped La2Mo2O7 compounds | |
| CN104250513B (en) | A kind of yellowish-brown near-infrared reflection type insulating moulding coating and preparation method thereof | |
| Geng et al. | Sol–gel combustion‐derived CoCuMnOx spinels as pigment for spectrally selective paints | |
| CN102618157B (en) | Infrared low-emissivity coating material and preparation method thereof | |
| CN102585572A (en) | Heat-reflecting heat-insulation inorganic composite material as well preparation method and application thereof | |
| Chen et al. | Sustainable cool pigments based on iron and tungsten co-doped lanthanum cerium oxide with high NIR reflectance for energy saving | |
| CN109384257A (en) | A kind of rare-earth pigment and its preparation method and application with high near infrared reflectivity | |
| CN104845428A (en) | Additive composition, thermal-insulation paint and application thereof | |
| Zeng et al. | Preparation and thermal reflectivity of nickel antimony titanium yellow rutile coated hollow glass microspheres composite pigment | |
| CN106497260A (en) | A kind of washability heat insulation exterior coating material and preparation method thereof | |
| Cao et al. | Preparation of phthalocyanine blue/rutile TiO2 composite pigment with a ball milling method and study on its NIR reflectivity | |
| CN106318162B (en) | Iron/nitrogen-doped titanic acid magnesium-based infrared composite material and preparation method thereof | |
| Xiao et al. | Synthesis and characterization of multi-colored pigments of LiRE (MoO4+ δ) 2 (RE= Ce, Pr, Nd, Er) with high near-infrared reflectance | |
| CN106336789B (en) | Iron/nitrogen-doped titanic acid cerium base infrared composite material and preparation method thereof | |
| CN106366875B (en) | Iron/nitrogen-doped titanic acid aluminium base infrared composite material and preparation method thereof | |
| CN104250514B (en) | A kind of dark-brown near-infrared reflection type insulating moulding coating and preparation method thereof | |
| CN106366878B (en) | Manganese/N doping aluminic acid zinc-base infrared composite material and preparation method thereof | |
| CN106349897B (en) | Bismuth/nitrogen-doped titanic acid aluminium base infrared composite material and preparation method thereof | |
| Zhang et al. | Environmentally Friendly High-Near-Infrared Reflectance Blue Pigment YIn0. 9–x Mn0. 1M x O3− δ Based on Li/Zn Doping | |
| CN108017936A (en) | A kind of preparation method of spherical compound ultra-fine yellow ceramic paint | |
| CN106318161B (en) | Cerium/nitrogen-doped titanic acid lanthanum base infrared composite material and preparation method thereof | |
| Xiong et al. | The far-infrared emissivity and near-infrared reflectance of Mg1-xMnxFe2O4 synthesized by xerogel-microwave method | |
| CN106243944B (en) | Cerium/nitrogen-doped titanic acid aluminium base infrared composite material and preparation method thereof | |
| CN107384072B (en) | Infrared-reflection heat-insulation coating and preparation method thereof based on bismuth molybdate compound | |
| CN106433336A (en) | Economical and environment-friendly external wall thermal insulating coating material and preparing method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190621 Termination date: 20210827 |