CN106634069A - Preparation method of brown material with low infrared emitting ability - Google Patents

Preparation method of brown material with low infrared emitting ability Download PDF

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Publication number
CN106634069A
CN106634069A CN201611038140.3A CN201611038140A CN106634069A CN 106634069 A CN106634069 A CN 106634069A CN 201611038140 A CN201611038140 A CN 201611038140A CN 106634069 A CN106634069 A CN 106634069A
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preparation
low infrared
chrome
water
infrared emissivity
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霍冀川
黄家建
雷永林
肖鹏
罗娟
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Southwest University of Science and Technology
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Southwest University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D1/00Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B25/00Phosphorus; Compounds thereof
    • C01B25/16Oxyacids of phosphorus; Salts thereof
    • C01B25/26Phosphates
    • C01B25/45Phosphates containing plural metal, or metal and ammonium
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18Fireproof paints including high temperature resistant paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/30Camouflage paints

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Inorganic Chemistry (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a preparation method of a brown material with low infrared emitting ability; the preparation method is characterized by comprising the following steps: taking 100 parts by mass of chrome-aluminum phosphate, placing the chrome-aluminum phosphate into a reactor and heating to 75 to 85 DEG C, adding 1 to 55 parts by mass of copper powder, reacting for 25 to 35min under the condition of stirring, then heating to 175 to 185 DEG C, and performing heat preservation and drying for 2.5 to 3.5h, thus obtaining the brown material with the low infrared emitting ability. By adopting the invention, the preparation method is simple, and the obtained Cu-chrome-aluminum phosphate based material with low infrared emitting ability has the characteristics that the material resists the heat as high as 1300 DEG C, the moisture absorption ratio is lowered to 0.05wt% minimally; the infrared emitting ability is lowered to 0.64 minimally, the performance is good and the material is suitable for being used as an infrared camouflage (stealth) coating.

Description

A kind of preparation method of brown low infrared emissivity material
Technical field
The invention belongs to the preparation of coating, is related to a kind of preparation method of brown low infrared emissivity material.Present invention system Standby brown low infrared emissivity material is particularly useful as infrared camouflage (stealthy) coating.
Background technology
Along with various investigative techniques such as the high speed development of national defence high and new technology, infrared detection, laser emission, radar detections From discovery so far, obtain the pro-gaze of countries in the world and use.International situation is continually changing, and war situation is more nervous, information Change war progressively to highlight, precision guided weapon then becomes the emphasis of countries in the world military technology development.Infrared acquisition guidance is military Device relies on its many advantage, including high accuracy, high sensitivity, high frame frequency, high-resolution, strong interference immunity, and have concurrently can Automatic identification target, can work double tides the features such as, seeker and ammunition are had been widely used at present.In addition, infrared imaging is visited Survey technology has distinctive advantage that is disguised, scouting the aspects such as precision, portability, reconnaissance range and anti-interference by it, Occupy space of prominence in various countries' military surveillance technology, be rapidly developed and be widely used in military affairs.Society Development accelerates the paces of scientific and technological progress, and the development of modern military technology is particularly swift and violent, various new military surveillance technologies and guidance The development of technology is maked rapid progress, and is emerged in an endless stream and input application rapidly, and the existence for making combatant and military target is subject to serious Threaten.In recent years countries in the world adopt infrared detection technique, its severity to reach this stage in local war:If mesh Mark thing is found that moment will be hit and be destroyed by infrared detection.If our the stealthy means in operation are poor, target will It is exposed, causes military combat personnel, military target, military weaponry etc. seriously to be threatened.Detect in infrared radar etc. System is woven on the modern battlefield of dragnet, it is necessary to is effectively hidden oneself, could be made the most of the advantage in operation, ability Obtain the hope of existence.Various military targets, especially moving target, such as guided missile, aircraft, aircraft carrier, warship, they Power source power it is big, ferocious infra-red radiation is easily produced during motion;The target of some high-speed motions, in motion process In, its shell and air frictional heat are also the source of infrared radiation.Infrared acquisition principle is complicated, mainly uses moving target itself The infra-red radiation of generation is the task such as completing to track, recognize, guide and attack.For near-infrared, the key of target exposure It is luminance difference of the target itself and background between, and mid-infrared, far main exposure symptoms are then temperature contrasts.
Infrared stealth technology is the emerging technology risen with infrared detection technique.By the structure for improving material Design and using Infrared Physics principle so that infrared energy is decayed or absorbed, reduce the target property visited.It is infrared hidden Body technology reduces the infrared intensity and characteristic of target using measures such as low-launch-rate coating, infrared shielding, heat suppression, Realize the low detectivity of military target.By reducing infrared intensity, changing infra red radiation band, adjust infra-red radiation Realizing infrared stealth technology, the research of low infrared emissivity coating is research thermal stealth coating to three aspects of transmitting procedure Crucial and difficult point.
In prior art, Britain《Jian Shi defence》Reported on 2 23rd, 2009:Internet companies develop and develop Infrared stealth coating technology, the electromagnetic wave transparent material for spraying 50 μ m-thicks just can be with limited target to thermal-radiating absorption and transmitting. G.Tricot is studied the thing phase change in aluminum phosphate solution temperature-rise period with method associated with XRD and nuclear-magnetism, to only Supplemented using the XRD analysis message to be provided.A kind of dielectric constant of the Nelson electric corporation research and development of Britain Between 4.5-7, dielectric loss angle tangent value be less than 0.0003, mainly with phosphate as this kind of material the nuclei of crystallization, Frequency obtained by its experiment, is mainly used in guided missile and other aircrafts with height both mechanically and thermally between 103Hz and 1010Hz Glass ceramics antenna house.It can be seen that, phosphate material is very wide in the application that national defense and military fields are obtained, if its emissivity can be reduced Extremely important impact will be produced for national defence stealth material.
The domestic research for infrared stealth coating is still in the primary research stage.
The low infrared emissivity material developed at present has the shortcomings that processing difficulties, high cost, stability are poor;It is existing infrared Oneself is formed with colorization to invisible coating, but also exist colored kind not enough enrich, in terms of physical and mechanical properties and workability The deficiencies such as, poor practicability incompatible with low-launch-rate.
The content of the invention
The purpose of the present invention is intended to overcome deficiency of the prior art, there is provided a kind of low cost, preparation process are simple, both have There is heat-resisting quantity that there is lower temperature resistance, the preparation method of brown low infrared emissivity material of good performance again.
Present disclosure is:A kind of preparation method of brown low infrared emissivity material, is characterized in that:Take chrome-alumina phosphate 100 mass parts, are placed in reactor and are heated to 75 DEG C~85 DEG C, add the mass parts of copper powder 1~55, and the lower reaction 25 of stirring~ 35min, then reacting rear material is warming up to into heat preservation and dryness 2.5h~3.5h at a temperature of 175 DEG C~185 DEG C, that is, brown is obtained low Infrared emittance material (or claim:Cu- chromium phosphate aluminium base low infrared emissivity materials).
In present disclosure:The preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.4~1.8:0.4~0.7:0.4~0.7:8~9 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al(OH)3], chromium trioxide (CrO3), methyl alcohol (CH3) and water (H OH2O);By the water of methyl alcohol and 1/8 amount (i.e.:Total consumption of water 1/8) be mixed into methanol aqueous solution;
Reaction:By the water of phosphoric acid and 7/8 amount (i.e.:7/8) mixing for total consumption of water, is heated to 75 DEG C~85 DEG C under stirring And it is incubated 5~8min;Add aluminium hydroxide, 25~35min of insulation reaction at 75 DEG C~85 DEG C;Chromium trioxide is added, 25~35min of insulation reaction at 75 DEG C~85 DEG C;Methanol aqueous solution is added dropwise to again, after dripping, then is protected at 75 DEG C~85 DEG C Warm 50~70min of stirring reaction, that is, be obtained (sticky shape is serpentinous) chrome-alumina phosphate;
In present disclosure:The consumption of the copper powder is preferably 25~30 mass parts.Copper powder addition is more, though favorably In infrared emittance is reduced, the reflection to radar wave, visible ray and laser is but increased, be unfavorable for laser, radar and visible ray It is stealthy.
In present disclosure:The particle diameter of the copper powder is preferably 0.1~100 μm.
Compared with prior art, the present invention has following features and beneficial effect:
(1) using aluminum phosphate chromium as matrix and adhesive, Ni metal powder is added in aluminum phosphate chromium to be made the present invention Its solidification, is obtained Cu- chromium phosphate aluminium base low infrared emissivity materials, the low infrared emissivity material high temperature resistant, up to 1300 DEG C, moisture absorption ratio is minimum to be down to 0.05wt%;Infrared emittance is minimum to drop to 0.64, can be in the form of infrared camouflage (stealthy) coating Various military targets are applied to, for example:The fields such as spacecraft, radar, guided missile, space station, assembling, in national defence, military affairs, new material Aspect has broad application prospects;
(2) using the present invention, copper had not only made curing agent but also had made filler, can both promote chrome-alumina phosphate solidification, reduce Its solidification temperature, can adjust infrared emittance and color as filler again, and aluminum phosphate chromium is easy to use, adhesive strength is high, resistance to High temperature, low temperature resistant, economical, environmental protection;
(3) using the obtained Cu- chromium phosphate aluminium base low infrared emissivity materials of the present invention, sent out by selecting suitable difference Penetrate the coating of rate and carry out design, target thermal image can be made to form image segmentation effect, eliminate the typical case of target thermal image Contour feature, reduces the recognition capability of thermal imaging system, obtains good thermal infrared stealth effect;
(4) raw material of the present invention is cheap, preparation process is simple, easily operation, and product cleanliness without any pollution is practical.
Description of the drawings
Fig. 1 be embodiment of the present invention infrared emittance with percentage of metal variation diagram, in Fig. 1, ordinate is infrared It is percentage of metal to penetrate rate, abscissa, and the percentage of metal refers to that copper powder quality accounts for the percentage of chrome-alumina phosphate quality Than that is,:Mass parts (g) X100% of copper powder mass parts (g)/chrome-alumina phosphate 100.
Specific embodiment
The invention will be further described for example given below plan, but is not to be construed as to the scope of the present invention Restriction, some nonessential improvement and tune that person skilled in art makes according to the content of the invention described above to the present invention It is whole, still fall within protection scope of the present invention.
Embodiment 1:
A kind of preparation method of brown low infrared emissivity material, step is as follows:
First, experimental section
1st, experimental raw:Using aluminium hydroxide [molecular formula Al (OH)3], phosphoric acid (molecular formula H3PO4), chromium trioxide (molecule Formula CrO3), methyl alcohol (molecular formula CH3OH), copper powder and water (can be ultra-pure water, distilled water or deionized water) carry out reality for raw material Test, each experimental raw is provided by Chengdu Ke Long chemical reagents factory;
2nd, laboratory apparatus:The model of the laboratory apparatus used during compound experiment and sample characterization and manufacturer are such as Shown in table 1 below.
Table 1:Major experimental instrument
Title Model Instrument provides enterprise
Electronic balance FA-1004 Shanghai Sunny Hengping Scientific Instrument Co., Ltd.
Collection heat examination constant-temperature heating magnetic stirring apparatus DF-101S Ya Rong Instrument Ltd. of Zhengzhou City
Reinforcement electric mixer JJ-1 Medical Instruments factory of Jintan City
Infrared emittance analyzer TSS-5X Beijing Hua Ruisen developments in science and technology Co., Ltd
3rd, experimentation
Chrome-alumina phosphate 100g is taken, is placed in reactor and is heated to 80 DEG C (can be with heating water baths), add copper powder 10g, stirring Reaction 30min, then reacting rear material is warming up to into heat preservation and dryness 3h at a temperature of 180 DEG C, that is, brown low infrared emissivity is obtained Material (or claim:Cu- chromium phosphate aluminium base low infrared emissivity materials).
2nd, infrared emittance is determined
1st, infrared emissivity tester device
The TSS-5X type infrared emittance instrument produced using Beijing Hua Ruisen developments in science and technology Co., Ltd, the infrared emittance The operation principle of instrument mainly uses the far infrared irradiation source of constant temperature radiation, reflected energy will be calculated after energy exposure.
2nd, infrared emittance assay method
By obtained brown low infrared emissivity material grind into powder, to powder pressed disc method process, diameter is prepared into To be tested after the circle sheet of Φ=30mm, measurement area is Φ=15mm, and measurement distance is the 12mm (pin of fixed detecting head Post portion).
3rd, data processing
Measured data are imported in drawing and DAS Origin8.0, infrared emittance is obtained with metal Changes of contents figure, as shown in figure 1, it is percentage of metal that ordinate is infrared emittance, abscissa, the percentage of metal is Refer to that copper powder quality accounts for the percentage of chrome-alumina phosphate quality, i.e.,:The mass parts of copper powder mass parts (g)/chrome-alumina phosphate 100 (g) X100%.
Embodiment 2~14:
A kind of preparation method of brown low infrared emissivity material, in embodiment 2~14, the preparation brown is low infrared The consumption of copper powder is corresponded to respectively in the step of penetrating rate material b:1g、3g、5g、10g、7g、15g、20g、25g、30g、35g、 40g, 45g, 50g and 55g;The other the same as in Example 1, omits.
Embodiment 15:
A kind of preparation method of brown low infrared emissivity material, step is:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 75 DEG C, add the mass parts of copper powder 1, the lower reaction 35min of stirring, then reacting rear material is warming up to into 175 DEG C At a temperature of insulation reaction 3.5h, that is, brown low infrared emissivity material is obtained and (or claims:The low infrared emission of Cu- chromium phosphate aluminium bases Rate material).
Embodiment 16:
A kind of preparation method of brown low infrared emissivity material, step is:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 85 DEG C, add the mass parts of copper powder 55, the lower reaction 25min of stirring, then reacting rear material is warming up to into 185 DEG C At a temperature of heat preservation and dryness 2.5h, that is, brown low infrared emissivity material is obtained and (or claims:The low infrared emission of Cu- chromium phosphate aluminium bases Rate material).
Embodiment 17:
A kind of preparation method of brown low infrared emissivity material, step is:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 80 DEG C, add the mass parts of copper powder 28, the lower reaction 30min of stirring, then reacting rear material is warming up to into 180 DEG C At a temperature of heat preservation and dryness 3h, that is, brown low infrared emissivity material is obtained and (or claims:Cu- chromium phosphate aluminium base low infrared emissivities Material).
Embodiment 18:
A kind of preparation method of brown low infrared emissivity material, step is:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 78 DEG C, add the mass parts of copper powder 25, the lower reaction 28min of stirring, then reacting rear material is warming up to into 178 DEG C At a temperature of heat preservation and dryness 2.8h, that is, brown low infrared emissivity material is obtained and (or claims:The low infrared emission of Cu- chromium phosphate aluminium bases Rate material).
Embodiment 19:
A kind of preparation method of brown low infrared emissivity material, step is:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 82 DEG C, add the mass parts of copper powder 30, the lower reaction 30min of stirring, then reacting rear material is warming up to into 182 DEG C At a temperature of heat preservation and dryness 3.2h, that is, brown low infrared emissivity material is obtained and (or claims:The low infrared emission of Cu- chromium phosphate aluminium bases Rate material).
Embodiment 20:
A kind of preparation method of brown low infrared emissivity material, step is:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 80 DEG C, add the mass parts of copper powder 27, the lower reaction 30min of stirring, then reacting rear material is warming up to into 180 DEG C At a temperature of heat preservation and dryness 3h, that is, brown low infrared emissivity material is obtained and (or claims:Cu- chromium phosphate aluminium base low infrared emissivities Material).
Embodiment 21:
A kind of preparation method of brown low infrared emissivity material, step is:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 80 DEG C, add the mass parts of copper powder 29, the lower reaction 30min of stirring, then reacting rear material is warming up to into 180 DEG C At a temperature of heat preservation and dryness 3h, that is, brown low infrared emissivity material is obtained and (or claims:Cu- chromium phosphate aluminium base low infrared emissivities Material).
Embodiment 22:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:With phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], chromium trioxide (CrO3), methyl alcohol (CH3) and water OH (H2O it is) raw material, weighs 500g (5.10 moles) phosphoric acid (H3PO4), 112.76g (1.45 moles) aluminium hydroxide [Al (OH)3]、 48.16g (0.48 mole) chromium trioxide (CrO3), 15.72g (0.49 mole) methyl alcohol (CH3OH), and 133.3g (7.41 rub You) and 20.5g (1.14 moles) water (H2O);By 15.72g (0.49 mole) methyl alcohol (CH3OH) with the water of 20.5g (1.14 moles) It is mixed into methanol aqueous solution;
Reaction:Phosphoric acid is mixed (be diluted) with the water of 133.3g, is heated under stirring 80 DEG C (can be with heating water baths) And it is incubated 5min;It is (slow) again to add aluminium hydroxide, insulation reaction 30min at 80 DEG C;It is (slow) again to add chromium trioxide, Insulation reaction 30min at 80 DEG C;The methanol aqueous solution is added dropwise to again, after dripping, then the insulated and stirred reaction at 80 DEG C 60min, that is, be obtained (sticky shape is serpentinous) chrome-alumina phosphate;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
Embodiment 23:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.4:0.4:0.4:8 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], chromium trioxide (CrO3), methyl alcohol (CH3) and water (H OH2O);By methyl alcohol (CH3OH) it is mixed into methanol aqueous solution with the water of 1/8 amount;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 75 DEG C are heated under stirring and 8min is incubated;It is (slow) again to add hydrogen Aluminum oxide, insulation reaction 35min at 75 DEG C;It is (slow) again to add chromium trioxide, insulation reaction 35min at 75 DEG C;Drip again Methanol aqueous solution is added, after dripping, then the insulated and stirred reaction 70min at 75 DEG C, that is, (sticky shape is serpentinous) phosphorus is obtained Sour chromium aluminium;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
Embodiment 24:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.8:0.7:0.7:9 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], chromium trioxide (CrO3), methyl alcohol (CH3) and water (H OH2O);By methyl alcohol (CH3OH) it is mixed into methanol aqueous solution with the water of 1/8 amount;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 85 DEG C are heated under stirring and 5min is incubated;It is (slow) again to add hydrogen Aluminum oxide, insulation reaction 25min at 85 DEG C;It is (slow) again to add chromium trioxide, insulation reaction 25min at 85 DEG C;Drip again Methanol aqueous solution is added, after dripping, then the insulated and stirred reaction 50min at 85 DEG C, that is, (sticky shape is serpentinous) phosphorus is obtained Sour chromium aluminium;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
Embodiment 25:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.6:0.5:0.5:8.5 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], three oxidation Chromium (CrO3), methyl alcohol (CH3) and water (H OH2O);By methyl alcohol (CH3OH) it is mixed into methanol aqueous solution with the water of 1/8 amount;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 80 DEG C are heated under stirring and 8min is incubated;It is (slow) again to add hydrogen Aluminum oxide, insulation reaction 30min at 80 DEG C;It is (slow) again to add chromium trioxide, insulation reaction 30min at 80 DEG C;Drip again Methanol aqueous solution is added, after dripping, then the insulated and stirred reaction 60min at 80 DEG C, that is, (sticky shape is serpentinous) phosphorus is obtained Sour chromium aluminium;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
Embodiment 26:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.5:0.5:0.5:8 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], chromium trioxide (CrO3), methyl alcohol (CH3) and water (H OH2O);By methyl alcohol (CH3OH) it is mixed into methanol aqueous solution with the water of 1/8 amount;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 78 DEG C are heated under stirring and 6min is incubated;It is (slow) again to add hydrogen Aluminum oxide, insulation reaction 28min at 78 DEG C;It is (slow) again to add chromium trioxide, insulation reaction 28min at 78 DEG C;Drip again Methanol aqueous solution is added, after dripping, then the insulated and stirred reaction 56min at 78 DEG C, that is, (sticky shape is serpentinous) phosphorus is obtained Sour chromium aluminium;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
Embodiment 27:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.8:0.6:0.6:9 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], chromium trioxide (CrO3), methyl alcohol (CH3) and water (H OH2O);By methyl alcohol (CH3OH) it is mixed into methanol aqueous solution with the water of 1/8 amount;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 82 DEG C are heated under stirring and 7min is incubated;It is (slow) again to add hydrogen Aluminum oxide, insulation reaction 30min at 82 DEG C;It is (slow) again to add chromium trioxide, insulation reaction 30min at 82 DEG C;Drip again Methanol aqueous solution is added, after dripping, then the insulated and stirred reaction 62min at 82 DEG C, that is, (sticky shape is serpentinous) phosphorus is obtained Sour chromium aluminium;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
Embodiment 28:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.7:0.5:0.5:8.5 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], three oxidation Chromium (CrO3), methyl alcohol (CH3) and water (H OH2O);By methyl alcohol (CH3OH) it is mixed into methanol aqueous solution with the water of 1/8 amount;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 80 DEG C are heated under stirring and 6min is incubated;It is (slow) again to add hydrogen Aluminum oxide, insulation reaction 30min at 80 DEG C;It is (slow) again to add chromium trioxide, insulation reaction 30min at 80 DEG C;Drip again Methanol aqueous solution is added, after dripping, then the insulated and stirred reaction 60min at 80 DEG C, that is, (sticky shape is serpentinous) phosphorus is obtained Sour chromium aluminium;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
Embodiment 29:
A kind of preparation method of brown low infrared emissivity material, the preparation method of the chrome-alumina phosphate is:
Dispensing:By phosphoric acid (H3PO4):Aluminium hydroxide [Al (OH)3]:Chromium trioxide (CrO3):Methyl alcohol (CH3OH):Water (H2O) =5.1:1.7:0.55:0.55:9 mol ratio takes each component raw material phosphoric acid (H3PO4), aluminium hydroxide [Al (OH)3], three oxidation Chromium (CrO3), methyl alcohol (CH3) and water (H OH2O);By methyl alcohol (CH3OH) it is mixed into methanol aqueous solution with the water of 1/8 amount;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 80 DEG C are heated under stirring and 7min is incubated;It is (slow) again to add hydrogen Aluminum oxide, insulation reaction 30min at 80 DEG C;It is (slow) again to add chromium trioxide, insulation reaction 30min at 80 DEG C;Drip again Methanol aqueous solution is added, after dripping, then the insulated and stirred reaction 60min at 80 DEG C, that is, (sticky shape is serpentinous) phosphorus is obtained Sour chromium aluminium;
Obtained chrome-alumina phosphate can be used for arbitrary in embodiment 1~21, omission.
In above-described embodiment:The particle diameter of the copper powder can be 0.1~100 μm.
In above-described embodiment:The each raw material for being adopted is commercially available prod.
In above-described embodiment:It is especially not dated in the percentage for being adopted, be quality (weight) percentage or Well known to a person skilled in the art percentage;Described quality (weight) part can be gram or kilogram.
In above-described embodiment:Technological parameter (temperature, time etc.) and each component numerical quantity in each step etc. are scope , any point is applicable.
The technology contents being not specifically delineated in present invention and above-described embodiment are compared with technology.
The invention is not restricted to above-described embodiment, can implement and with the good result described in present invention.

Claims (5)

1. a kind of preparation method of brown low infrared emissivity material, is characterized in that:The mass parts of chrome-alumina phosphate 100 are taken, is placed in anti- Answer and be heated in device 75 DEG C~85 DEG C, add the mass parts of copper powder 1~55, stirring 25~35min of lower reaction, then by reacting rear material Heat preservation and dryness 2.5h~3.5h at a temperature of 175 DEG C~185 DEG C is warming up to, that is, brown low infrared emissivity material is obtained.
2. as described in claim 1 brown low infrared emissivity material preparation method, it is characterized in that:The system of the chrome-alumina phosphate Preparation Method is:
Dispensing:By phosphoric acid:Aluminium hydroxide:Chromium trioxide:Methyl alcohol:Water=5.1:1.4~1.8:0.4~0.7:0.4~0.7:8~ 9 mol ratio takes each component raw material phosphoric acid, aluminium hydroxide, chromium trioxide, first alcohol and water;Methyl alcohol is mixed into the water of 1/8 amount Methanol aqueous solution;
Reaction:Phosphoric acid is mixed with the water of 7/8 amount, 75 DEG C~85 DEG C are heated under stirring and 5~8 min are incubated;Add hydrogen Aluminum oxide, the min of insulation reaction 25~35 at 75 DEG C~85 DEG C;Chromium trioxide is added, is incubated at 75 DEG C~85 DEG C anti- Answer 25~35min;Methanol aqueous solution is added dropwise to again, after dripping, then the insulated and stirred reaction 50~70 at 75 DEG C~85 DEG C Min, that is, be obtained chrome-alumina phosphate.
3. as described in claim 1 or 2 brown low infrared emissivity material preparation method, it is characterized in that:The use of the copper powder Measure as 25~30 mass parts.
4. as described in claim 1 or 2 brown low infrared emissivity material preparation method, it is characterized in that:The grain of the copper powder Footpath is 0.1~100 μm.
5. as described in claim 3 brown low infrared emissivity material preparation method, it is characterized in that:The particle diameter of the copper powder is 0.1~100 μm.
CN201611038140.3A 2016-11-23 2016-11-23 Preparation method of brown material with low infrared emitting ability Pending CN106634069A (en)

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