CN102627874A - Composite-structure pigment having low lightness and infrared emitting ability and preparation method thereof - Google Patents

Composite-structure pigment having low lightness and infrared emitting ability and preparation method thereof Download PDF

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CN102627874A
CN102627874A CN 201210072246 CN201210072246A CN102627874A CN 102627874 A CN102627874 A CN 102627874A CN 201210072246 CN201210072246 CN 201210072246 CN 201210072246 A CN201210072246 A CN 201210072246A CN 102627874 A CN102627874 A CN 102627874A
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aluminum
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卢虎
翁小龙
袁乐
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电子科技大学
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Abstract

The invention discloses a composite-structure pigment having low lightness and infrared emitting ability and a preparation method thereof, and belongs to the technical field of functional materials. The composite-structure pigment is aluminum powder of which particle surfaces are coated with nanoscale chromium oxide particles. The nanoscale chromium oxide particles hide the metal luster of particle surfaces of the aluminum powder so that a high infrared emitting ability of the aluminum powder is reduced suitably and thus the composite-structure pigment having low lightness and infrared emitting ability is obtained. The preparation method realizes deposition of nanoscale chromium oxide particles on particle surfaces of aluminum powder by a chemical precipitation method and a calcination process. The composite-structure pigment obtained by the preparation method has low lightness of 72.1 to 53.6 and infrared emitting ability of (0.71 to 0.43) in an atmospheric sounding window range of 8 to 14 microns, and can be used as a main padding of a multi-band (visible light band and infrared band) infrared camouflage coating.

Description

一种低明度和低红外发射率复合结构颜料及其制备方法 A low-brightness and low infrared emissivity and the composite structure of the pigment preparation

技术领域 FIELD

[0001] 本发明属于功能材料技术领域,涉及节能材料,尤其是适用于节能装饰涂料。 [0001] The present invention belongs to the technical field of functional materials, relates to energy-saving materials, particularly suitable for energy-saving decorative coatings. 发明包含一种具有低明度和红外低发射率复合颜料及其制备方法。 Invention include one having a low lightness and low infrared emissivity composite pigment preparation thereof. 背景技术 Background technique

[0002] 随着工业生产的快速发展,能源问题带来的矛盾在现代社会日益突出。 [0002] With the rapid development of industrial production, energy problems caused by increasingly prominent in modern society. 人们也越发提倡高效集约的使用能源。 It also advocated more intensive and efficient use of energy. 采用环保节能材料和技术能够有效提高能源的利用效率。 Green energy using materials and techniques can improve energy efficiency. 在不远的将来,节能材料的广泛使用将是一种重要趋势。 In the near future, widespread use of energy-saving materials will be an important trend.

[0003] 因为铝具有价格低廉、延展性、密度小等优点,微米级铝粉被广泛用作普通涂层的颜料。 [0003] Since aluminum has a low price, ductility, low density, etc., micron sized aluminum powder is widely used as a coating pigment common. 金属铝对红外辐射波和可见光的高反射特性,可能使其成为一种在未来被广泛使用的节能材料。 Aluminum high reflection property for the visible light and infrared radiation waves, the material may make it a widely used energy in the future. 如采用含铝粉颜料的装饰涂层能够有效减少建筑外立面对太阳辐射波的吸收,降低建筑物表面热量的聚集,对建筑物起到隔热保温的作用。 The use of a decorative coating containing the aluminum pigment can be effectively reduced absorption of solar radiation facade waves, reduce aggregation of the surface heat buildings, the building acts as heat insulation. 较高的热红外反射率也使铝粉成为一种重要的红外伪装填料。 High thermal infrared reflectivity aluminum powder also become an important infrared camouflage filler. 如上世纪八十年代起,西方国家都在红外隐身涂料中加入大量铝箔片,以降低目标红外发射率。 As from the eighties, the Western countries have joined a large number of aluminum foil in the infrared stealth coating in order to reduce the target infrared emissivity.

[0004] 铝粉在装饰涂料和红外伪装涂层中的应用空间主要受限于铝的颜色泛白、高金属光泽等特性。 [0004] In the application space aluminum and decorative coatings infrared camouflage coating of aluminum is mainly limited by the color white, high metallic gloss properties. 为了克服应用中的缺陷,通常的做法是在涂料中添加着色颜料以掩盖铝粉的光泽并调制涂层的颜色。 In order to overcome the deficiencies of applications, it is common practice to add a coloring pigment in the paint to conceal the aluminum gloss and color modulation of the coating. 但着色颜料通常具有的红外高发射特性使得涂层的红外低发射性能下降。 However, the coloring pigment generally has a high infrared emission characteristics such that the coating is a low infrared emission performance.

[0005]因此,一种具有低光泽、红外低发射、较好着色力特性的填料将具有广阔的应用前景。 [0005] Thus, with a low gloss, low infrared emission, a colored filler is preferably force characteristic will have broad application prospects. 将一种小颗粒材料包覆在另一种材料的大颗粒基体表面,制备核壳结构的复合材料,可使复合材料兼具两种材料的性能。 The coated particulate material in a small-granular matrix surface of another material, a composite material prepared core-shell structure, composite materials can both the properties of the two materials. 根据朗伯定律: According to Lambert's law:

Figure CN102627874AD00031

[0007] 其中a为均匀介质的吸收系数,k为消光系数。 [0007] wherein A is a homogeneous medium absorption coefficient, k is the extinction coefficient. 公式(I)表明辐射光穿过厚度为d的介质时,其辐射强度I会呈指数衰减,但同一介质对不同波长的辐射吸收效率存在巨大的差异:辐射的波长越短,介质对其的吸收系数越高。 When the formula (I) show radiation through the thickness d of the medium, the radiation intensity I will exponentially decay, but a huge difference in the same media in the radiation absorption efficiency of different wavelengths: the shorter the wavelength of the radiation medium thereof The higher the absorption coefficient. 根据上式,只需合理控制铝片表面颗粒包覆层的厚度,红外光就能以较小的损耗穿过颗粒层到达铝片表面,从而保持高红外反射率;波长较短的可见光穿透介质时大部分被介质损耗,使得材料的明度降低。 According to the above formula, the thickness of the aluminum foil only reasonable control of the coating layer surface of the particles, the infrared light can pass through the particles with a small loss of surface layer to the aluminum sheet, thus maintaining a high infrared reflectivity; shorter wavelength visible light passing when most of the medium dielectric loss material such that the brightness is reduced. 最终实现复合材料的红外低发射、低明度特性。 IR ultimately composite low emissivity, low illuminance characteristics.

发明内容 SUMMARY

[0008] 本发明提供一种低明度和低红外发射率复合结构颜料,所述复合结构颜料为一种表面包覆纳米氧化铬颗粒的铝粉,利用纳米氧化铬颗粒遮盖铝粉表面的金属光泽,适当降低铝粉的高红外反射能力,从而得到低明度和低红外发射率的复合结构颜料。 [0008] The present invention provides a low brightness and low infrared emissivity of the composite structure of the pigment, the composite structure of the pigment-coated aluminum nano-particles is a surface-chromium oxide, chromium oxide nano-particles using aluminum covers the surface of the metallic luster , due to lower aluminum high infrared reflectivity, to give a composite structure of the pigment and the low brightness is the low infrared emissivity. 所述复合结构颜料由于具有较低的明度和红外发射率,使得该复合结构颜料可作为多波段(可见光与红外波段)红外伪装涂料的主体填料用。 Since the composite structure has a lower pigment brightness and infrared emissivity, such that the composite structure of the pigment can be used as a multi-band (visible and infrared) IR camouflage paint body with a filler. 本发明同时提供该复合结构颜料的制备方法,该方法采用化学沉淀法加煅烧工艺在铝粉表面沉积纳米氧化铬颗粒,具有成本低廉、易于实现的特点。 The present invention also provides a method of preparing the composite structure of the pigment, the method using chemical precipitation process of adding the calcined chromium oxide nano-particles deposited aluminum surface, having a low cost, easy implementation.

[0009] 本发明的实质是将一种小颗粒材料附着在另一种材料的大颗粒基体表面,制备核壳结构的复合材料,使复合材料兼具两种材料的性能。 [0009] The essence of the invention is a small-large particles in the particulate material adhered to the substrate surface of another material, making a composite core-shell structure, composite materials with the properties of the two materials. 在片状铝粉表面附着氧化铬颗粒,降低铝粉的反光特性,同时对铝粉的低红外发射特性影响较小。 Chromium oxide adhered aluminum flake particles, to reduce the reflective properties of the aluminum, while little effect on the properties of low infrared emissivity of aluminum.

[0010] 本发明技术方案如下: [0010] aspect of the present invention is as follows:

[0011] 一种低明度和低红外发射率复合结构颜料,包括片状铝粉和包覆于片状铝粉表面的纳米氧化铬颗粒,采用如下方法制备: [0011] A low lightness and low infrared emissivity of the composite structure of the pigment comprising aluminum flakes and chromium oxide nano-particles coated on the surface of the aluminum flakes, prepared using the following method:

[0012] 步骤I :采用粒径在I〜50微米的漂浮型片状铝粉,用无水乙醇将铝粉泡开并溶解其表面有机物,清洗、过滤、干燥后得到纯净的片状铝粉。 [0012] Step I: In the use of particle size of aluminum flakes floating I~50 microns, with anhydrous ethanol and dissolved aluminum soaked surface organics, washed, filtered and dried to give pure aluminum flakes .

[0013] 步骤2 :将Cr(NO3)3 • 9H20溶于无水乙醇,控制Cr离子浓度在0. 03〜0. 2M之间。 [0013] Step 2: Cr (NO3) 3 • 9H20 were dissolved in ethanol, controlling the Cr ion concentration between 0. 03~0 2M..

[0014] 步骤3 :将步骤I所得纯净的片状铝粉、步骤2所得Cr (NO3)3 • 9H20的无水乙醇溶液和乳化剂0P-10混合,控制混合体系中Cr(NO3)3 • 9H20与片状铝粉的摩尔比在(0. 04〜 [0014] Step 3: Step I obtained pure aluminum flake, Step 2 resulting Cr (NO3) 3 • 9H20 absolute ethanol and mixed emulsifier 0P-10, control of the hybrid system Cr (NO3) 3 • 9H20 molar ratio of the aluminum flakes (0. 04~

1.0) : I 之间。 1.0): between I.

[0015] 步骤4 :将步骤3所得混合体系置于20〜70°C环境下搅拌反应,搅拌反应过程中滴加无水乙醇稀释的碱性溶液,使混合体系PH值保持在7〜9之间;反应完毕后收集沉淀,并经清洗、干燥、研磨得到表面包覆Cr(OH)3的片状铝粉。 [0015] Step 4: The mixture obtained in Step 3 The reaction system is placed stirred at 20~70 ° C environment, the reaction was stirred during the dropwise addition of anhydrous ethanol diluted alkaline solution, the combined system is maintained at the PH value 7~9 of Room; after completion of the reaction the precipitate was collected, washed and dried, dried, milled to obtain surface-coated Cr (OH) 3 aluminum flakes.

[0016] 步骤5 :将步骤4所得表面包覆Cr (OH) 3的片状铝粉置于400〜450°C环境下煅烧处理,得到表面包覆纳米氧化铬颗粒的片状铝粉,即低明度和低红外发射率的复合结构颜料。 [0016] Step 5: The step of coating the surface 4 resulting Cr (OH) 3 was placed in aluminum flakes calcination treatment at 400~450 ° C environment, the surface-coated aluminum flakes obtained chromium oxide nano-particles, i.e., the composite structure of the pigment and the low brightness is the low infrared emissivity.

[0017] 上述技术方案中,为了防止纳米氧化铬颗粒在片状铝粉表面团聚,提高氧化铬颗粒在片状铝粉表面的分散性,在对步骤4所得表面包覆Cr(OH)3的片状铝粉进行步骤5所述煅烧处理之前,可先对步骤4所得表面包覆Cr (OH) 3的片状铝粉进行水热处理,具体水热处理温度在150〜200°C之间,时间为4〜24小时。 [0017] In the above technical solutions, in order to prevent chromium oxide nano-particles in the aluminum flake agglomeration, to improve the dispersibility of the chromia particles in the aluminum flake coated Cr (OH) 4 obtained in step 3 of the surface before firing the aluminum flake five step process, the first coating may be Cr (OH) 3 aluminum flakes hydrothermal treatment obtained in step 4 of the surface, particularly the hydrothermal treatment at a temperature between 150~200 ° C, time It is 4~24 hours.

[0018] 一种低明度和低红外发射率复合结构颜料的制备方法,如图I所示,包括以下步骤: [0018] A low lightness and low infrared emissivity of producing a composite structure of the pigment, as shown in FIG. I, comprising the steps of:

[0019] 步骤I :采用粒径在I〜50微米的漂浮型片状铝粉,用无水乙醇将铝粉泡开并溶解其表面有机物,清洗、过滤、干燥后得到纯净的片状铝粉。 [0019] Step I: In the use of particle size of aluminum flakes floating I~50 microns, with anhydrous ethanol and dissolved aluminum soaked surface organics, washed, filtered and dried to give pure aluminum flakes .

[0020] 步骤2 :将Cr (NO3) 3 • 9H20溶于无水乙醇,控制Cr离子浓度在0. 03〜0. 2M之间。 [0020] Step 2: Cr (NO3) 3 • 9H20 were dissolved in ethanol, controlling the Cr ion concentration between 0. 03~0 2M..

[0021] 步骤3 :将步骤I所得纯净的片状铝粉、步骤2所得Cr(NO3)3 • QH2O的无水乙醇溶液和乳化剂0P-10混合,控制混合体系中Cr(NO3)3 • 9H20与片状铝粉的摩尔比在(0. 04〜 [0021] Step 3: Step I obtained pure aluminum flake, Step 2 resulting Cr (NO3) 3 • QH2O of absolute ethanol and mixed emulsifier 0P-10, control of the hybrid system Cr (NO3) 3 • 9H20 molar ratio of the aluminum flakes (0. 04~

1.0) : I 之间。 1.0): between I.

[0022] 步骤4 :将步骤3所得混合体系置于40〜70°C环境下搅拌反应,搅拌反应过程中滴加碱性乙醇溶液,使混合体系PH值保持在7〜9之间;反应完毕后收集沉淀,并经清洗、干燥、研磨得到表面包覆Cr(OH)3的片状铝粉。 [0022] Step 4: The mixture obtained in Step 3 The reaction system is placed stirred at 40~70 ° C environment, the reaction was stirred during the dropwise addition of an alkaline solution of ethanol, the combined system is held between the PH value 7~9; completion of the reaction after the precipitate was collected, washed and dried, dried, milled to obtain surface-coated Cr (OH) 3 aluminum flakes.

[0023] 步骤5 :将步骤4所得表面包覆Cr (OH) 3的片状铝粉置于400〜450°C环境下煅烧处理,得到表面包覆纳米氧化铬颗粒的片状铝粉,即低明度和低红外发射率的复合结构颜料。 [0023] Step 5: The step of coating the surface 4 resulting Cr (OH) 3 was placed in aluminum flakes calcination treatment at 400~450 ° C environment, the surface-coated aluminum flakes obtained chromium oxide nano-particles, i.e., the composite structure of the pigment and the low brightness is the low infrared emissivity.

[0024] 上述技术方案中,为了防止纳米氧化铬颗粒在片状铝粉表面团聚,提高氧化铬颗粒在片状铝粉表面的分散性,在对步骤4所得表面包覆Cr(OH)3的片状铝粉进行步骤5所述煅烧处理之前,可先对步骤4所得表面包覆Cr (OH) 3的片状铝粉进行水热处理,具体水热处理温度在150〜200°C之间,时间为4〜24小时。 [0024] In the above technical solutions, in order to prevent chromium oxide nano-particles in the aluminum flake agglomeration, to improve the dispersibility of the chromia particles in the aluminum flake coated Cr (OH) 4 obtained in step 3 of the surface before firing the aluminum flake five step process, the first coating may be Cr (OH) 3 aluminum flakes hydrothermal treatment obtained in step 4 of the surface, particularly the hydrothermal treatment at a temperature between 150~200 ° C, time It is 4~24 hours.

[0025] 步骤3中所述混合体系的Cr (NO3) 3 • 9H20与片状铝粉的摩尔比应控制在(0. 04〜 [0025] Cr Step 3 in the mixing system (NO3) 3 • 9H20 and the molar ratio of aluminum flakes should be controlled (0. 04~

1.0) : I之间,铝粉和Cr(NO3)3的比例过高时,铝粉表面附着的颗粒较少,无法降低铝粉的明度值;铝粉和Cr(N03)3的比例过低时,最终生成的氧化铬颗粒团聚严重,并堆积在铝粉表面,使得粉体的发射率急剧升高。 1.0): between I, aluminum powder and Cr (NO3) 3 When the ratio is too high, small particles adhering to the surface of the aluminum powder, the aluminum powder can not be reduced brightness values; ratio of aluminum powder and Cr (N03) 3 is too low when, finally generated chromia severe particle agglomeration, and aluminum deposited on the surface, so that a sharp increase in emission of the powder.

[0026] 步骤4中所述碱性乙醇溶液为氢氧化钠的乙醇溶液或氨水的乙醇溶液。 The alkaline solution in ethanol [0026] Step 4 in ethanol is an ethanol solution of sodium hydroxide or aqueous ammonia solution. 步骤4中混合体系的PH值若低于7无法提供反应用的0H—1根离子,若pH值高于9,微米级的片状铝粉因为有很高的比表面积、活性较高,会和OIT1反应,在铝表面生成氢氧化铝。 The step of mixing PH value below 7. If the system can not provide 4 0H-1 ion reaction, if the pH value is higher than 9, since the micron-sized aluminum flakes have a high specific surface area, higher activity, will and OIT1 reaction to produce aluminum hydroxide in the aluminum surface. 在添加碱性乙醇溶液时,混合体系应控制在40°C〜70°C,并进行搅拌,低于40°C的温度需要加压,过高的温度则会导致无水乙醇的过度挥发,严重改变反应条件。 An alkaline solution upon addition of ethanol, mixing system should be controlled at 40 ° C~70 ° C, and with stirring, the temperature of 40 ° C lower than the required pressure, too high a temperature will result in excessive volatilization of ethanol, seriously changing the reaction conditions.

[0027] 采用本发明的方法制备的低明度和红外低发射率复合结构颜料,在8〜14微米的波长范围内,其红外发射率通常低于0. 7 (最低可达0. 43),明度值通常低于72 (最低可达50以下),表面几乎没有金属光泽。 [0027] Preparation of low brightness using methods of the present invention and the low emissivity infrared composite structure of the pigment in the wavelength range of 8~14 micrometers, the infrared emissivity is generally lower than 0.7 (as low as 0.43), lightness value is generally lower than 72 (as low as 50 or less), a surface almost no metallic luster. 根据可见光和红外伪装关注的不同,采用本发明可以制备发射率在0. 7〜0. 43,相应明度值范围在47. 7〜53. 6的表面附着不同含量氧化铬和具有不同形貌的铝粉改性颜料。 Depending on the visible and infrared camouflage of interest, the present invention can be prepared emissivity 0. 7~0. 43, the range of brightness values ​​corresponding to different amounts of attached chromium oxide and having a different surface topography 47. 7~53. 6 modified aluminum powder pigment. 本发明的表面包覆氧化铬的片状铝粉颜料具备以下的效果:红外发射率低,基本满足红外伪装的要求;明度低,基本没有金属反光;进过水热处理有很好的分散性,易于作为涂料的填料使用;进过高温煅烧后,颜料具有很好的稳定性。 Chromium oxide surface-coated aluminum flake pigment of the invention has the following effects: low IR emissivity, infrared camouflage basically meet the requirements; low brightness, substantially no metal reflector; into the water have a good heat dispersion, Ease of use as a paint filler; after high temperature calcination been to pigment having good stability.

附图说明 BRIEF DESCRIPTION

[0028] 图I即本发明流程示意图。 [0028] Figure I a schematic view of the present invention i.e. the process.

[0029] 图2为本发明作制备的低明度和低红外发射率复合结构颜料(表面包覆纳米氧化铬颗粒的片状铝粉)的扫描电镜图。 [0029] FIG. 2 is prepared as a low lightness and low infrared emissivity of the composite structure of the pigment (aluminum flake coated with chromium oxide nano-particles) of scanning electron micrographs invention.

具体实施方式 detailed description

[0030] 实施例I [0030] Example I

[0031] 按表I的摩尔比称取清洁的片状铝粉(粒径为8um)和Cr (NO3) 3 • 9H20并加入乳化剂0P-10 —起放入锥形瓶中,注入无水乙醇,控制Cr3+离子浓度为0. 07M ;将上述混合体系超声分散,并放入恒温水浴磁力搅拌器中搅拌;控制混合体系反应温度为60°C,缓慢滴加用无水乙醇稀释过的氨水溶液,使混合体系pH值控制在7〜9之间;待反应结束后,将制得的产物用离心机在2000r/min离心2分钟,滤去上层清液,沉淀物清洗、过滤后在50°C的恒温干燥箱干燥10个小时,得到的干燥粉体用玛瑙研钵研磨、晒网过筛后放入马弗炉中,在400〜450°C的温度条件下煅烧2小时,得到最终的低明度和低红外发射率的复合结构颜料。 [0031] The molar ratio of Table I Weigh cleaned aluminum flakes (particle diameter 8um) and Cr (NO3) 3 • 9H20 and an emulsifying agent 0P-10 - play into conical flask, anhydrous injection ethanol, Cr3 + ion concentration control of 0. 07M; the mixed ultrasonic dispersion system, placed in a thermostatic water bath and stirred on a magnetic stirrer; a control system in the reaction mixture temperature is 60 ° C, diluted with ethanol was slowly added dropwise over ammonia an aqueous solution of the mixed system pH was controlled between 7~9; after completion of the reaction, the obtained product was centrifuge at 2000r / min and centrifuged for 2 minutes, and the supernatant was removed by filtration, the precipitate was washed and filtered at 50 drying oven thermostat ° C. for 10 hours to give dried milled powder using an agate mortar, placed in a muffle furnace and after drying mesh screened, calcined at a temperature of 400~450 ° C for 2 hours, to give a final the composite structure of the pigment of low lightness and low infrared emissivity. 实验中铝粉由日本东洋公司生产,其他试剂均为分析纯。 Experiments in aluminum powder manufactured by Toyo Corporation, other reagents were of analytical grade. 最终产品的红外发射率和明度值如表I所示。 Infrared emissivity of the final product and the lightness value as shown in Table I.

[0032]表 I [0032] TABLE I

[0033] [0033]

Figure CN102627874AD00061

[0034] 实施例2 [0034] Example 2

[0035] 依据表2选取不同摩尔浓度的Cr(NO3)3 • 9H20的乙醇溶液,按照Cr(NO3)3 * 9H20 : Al摩尔比为0.1 : I加入清洁片状铝粉、并加入乳化剂0P-10 —起放入锥形瓶;将上述混合体系超声分散,并放入恒温水浴磁力搅拌器中搅拌;控制混合体系反应温度为60°C,缓慢滴加用无水乙醇稀释过的氨水溶液,使混合体系pH值控制在7〜9之间;待反应结束后,将制得的产物用离心机在2000r/min离心2分钟,滤去上层清液,沉淀物清洗、过滤后在50°C的恒温干燥箱干燥10个小时,得到的干燥粉体用玛瑙研钵研磨、晒网过筛后放入马弗炉中,在恒定的温度400〜450°C煅烧2小时,得到最终的低明度和低红外发射率的复合结构颜料。 [0035] according to Table 2 to select different molar concentrations of Cr (NO3) 3 • 9H20 in ethanol, according to the 3 * 9H20 Cr (NO3): Al molar ratio of 0.1: I added clean aluminum flake, and an emulsifier is added 0P -10-- onwards into the conical flask; the mixed ultrasonic dispersion system, placed in a thermostatic water bath and stirred on a magnetic stirrer; a control system in the reaction mixture temperature is 60 ° C, diluted with ethanol was slowly added dropwise over a solution of aqueous ammonia , the combined system pH was controlled between 7~9; after completion of the reaction, the obtained product was centrifuge at 2000r / min and centrifuged for 2 minutes, and the supernatant was removed by filtration, the precipitate was washed and filtered at 50 ° C constant temperature drying oven of 10 hours, the dried powder was ground with an agate mortar, placed in a muffle furnace and after drying mesh screened, calcined at a constant temperature of 400~450 ° C 2 hours to give a final low composite pigments lightness and low infrared emissivity. 实验中铝粉由日本东洋公司生产,其他试剂均为分析纯。 Experiments in aluminum powder manufactured by Toyo Corporation, other reagents were of analytical grade. 最终产品的发射率和明度值如表2所示。 The final product brightness value and the emissivity are shown in Table 2 below.

[0036]表 2 [0036] TABLE 2

[0037] [0037]

Figure CN102627874AD00062

[0038] 实施例3 [0038] Example 3

[0039] 依据表3选取不同粒径的清洁片状铝粉,按照Al : Cr(NO3)3WH2O摩尔比为0.1 : I加入Al : Cr(NO3)3 *9H20的乙醇溶液,并加入乳化剂0P-10—起放入锥形瓶配置溶液,控制Cr3+离子浓度为0. 07M ;将上述混合体系超声分散,放入恒温水浴磁力搅拌器中搅拌;控制混合体系的反应温度为60°C,缓慢滴加用无水乙醇稀释过的氨水溶液,使混合体系PH值控制在7〜9之间;待反应结束后,将制得的产物用离心机在2000r/min离心2分钟,滤去上层清液,沉淀物清洗、过滤后在50°C的恒温干燥箱干燥10个小时,得到的干燥粉体用玛瑙研钵研磨、晒网过筛后放入马弗炉中,在恒定的温度400〜450°C煅烧2小时,得到最终的低明度和低红外发射率的复合结构颜料。 [0039] Table 3 based on selection of different particle sizes of aluminum flakes cleaned according to Al: 3WH2O molar ratio of Cr (NO3) is 0.1: I added Al: Cr (NO3) 3 * 9H20 in ethanol and adding an emulsifier 0P -10- arranged from solution into the conical flask, the control Cr3 + ion concentration 0. 07M; the mixed ultrasonic dispersion system, placed in a thermostatic water bath with stirring on a magnetic stirrer; the reaction mixture temperature control system is 60 ° C, slowly dropwise with absolute ethanol diluted ammonia solution, the combined system control between the PH value 7~9; after completion of the reaction, the obtained product was centrifuge at 2000r / min and centrifuged for 2 minutes, and the supernatant was filtered off liquid, washing the precipitate, drying oven at a constant temperature of 50 ° C after 10 hours was filtered, dried powder was ground with an agate mortar, placed in a muffle furnace and after drying mesh sieve, at a constant temperature of 400~ 450 ° C calcined for 2 hours, to give the final structure of the pigment composite low illuminance and low infrared emissivity. 实验中铝粉由日本东洋公司生产,其他试剂均为分析纯。 Experiments in aluminum powder manufactured by Toyo Corporation, other reagents were of analytical grade. 最终产品的发射率和明度值如表3所示。 The final product emissivity and brightness values ​​as shown in Table 3.

[0040]表 3 [0040] TABLE 3

[0041] [0041]

Figure CN102627874AD00063

Claims (6)

  1. 1. ー种低明度和低红外发射率复合结构颜料,包括片状铝粉和包覆于片状铝粉表面的纳米氧化铬颗粒,采用如下方法制备: 步骤I :采用粒径在I〜50微米的漂浮型片状铝粉,用无水こ醇将铝粉泡开并溶解其表面有机物,清洗、过滤、干燥后得到纯净的片状铝粉; 步骤2 :将Cr (NO3) 3 · 9H20溶于无水こ醇,控制Cr离子浓度在O. 03〜O. 2M之间; 步骤3 :将步骤I所得纯净的片状铝粉、步骤2所得Cr(NO3)3 ·9Η20的无水こ醇溶液和乳化剂0Ρ-10混合,控制混合体系中Cr (NO3) 3 ·9Η20与片状铝粉的摩尔比在(O. 04〜I. O) : I之间; 步骤4 :将步骤3所得混合体系置于20〜70°C环境下搅拌反应,搅拌反应过程中滴加无水こ醇稀释的碱性溶液,使混合体系pH值保持在7〜9之间;反应完毕后收集沉淀,并经清洗、干燥、研磨得到表面包覆Cr(OH)3的片状铝粉; 步骤5 :将步骤4所得表面包覆Cr (OH) 3 1. ー kinds of low brightness and low infrared emissivity of the composite structure of the pigment comprising aluminum flakes and chromium oxide nano-particles coated on the aluminum flake prepared using the following method: Step I: particle size using I~50 leafing aluminum flakes microns, with anhydrous aluminum ko ol surface soaked and dissolved organics, washed, filtered and dried to give pure aluminum flake; step 2: Cr (NO3) 3 · 9H20 ko was dissolved in anhydrous alcohol, Cr ion concentration control O. 03~O between 2M; step 3: the step I obtained pure aluminum flakes, the resulting Cr 2 step (of NO3) 3 · 9Η20 of anhydrous ko alcohol solution and mixed emulsifier 0Ρ-10, control of the hybrid system 3 · 9Η20 molar ratio of aluminum flakes and Cr (NO3) in (O. 04~I O.): between I; step 4: step 3 the resulting mixture was stirred system was placed under the reaction environment 20~70 ° C, the reaction was stirred during the dropwise over anhydrous ko alcohol alkaline solution is diluted, the pH of the combined system was maintained between 7~9; after completion of the reaction the precipitate is collected, and cleaned, dried and ground to obtain surface-coated Cr (OH) 3, aluminum flakes; step 5: the step of coating the surface 4 resulting Cr (OH) 3 片状铝粉置于400〜450°C环境下煅烧处理,得到表面包覆纳米氧化铬颗粒的片状铝粉,即低明度和低红外发射率的复合结构颜料。 Aluminum flake placed calcination treatment at 400~450 ° C environment, the surface-coated aluminum flakes obtained chromium oxide nano-particles, i.e., the composite structure of the pigment of low lightness and low infrared emissivity.
  2. 2.根据权利要求I所述的低明度和低红外发射率复合结构颜料,其特征在于,在对步骤4所得表面包覆Cr (OH) 3的片状铝粉进行步骤5所述煅烧处理之前,先对步骤4所得表面包覆Cr(OH)3的片状铝粉进行水热处理,具体水热处理温度在150〜200°C之间,时间为4〜24小时。 The low brightness and low infrared emissivity of the composite pigment as claimed in claim I, wherein the coated Cr (OH) 3 aluminum flakes 5 the calcining process is performed in step 4 prior to step resulting surface , first coated Cr (OH) 3 aluminum flakes hydrothermal treatment obtained in step 4 of the surface, particularly the hydrothermal treatment at a temperature between 150~200 ° C, time of 4~24 hours.
  3. 3.根据权利要求I所述的低明度和低红外发射率复合结构颜料,其特征在于,步骤4中所述碱性こ醇溶液为氢氧化钠的こ醇溶液或氨水的こ醇溶液。 The low brightness and low infrared emissivity of the composite pigment as claimed in claim I, wherein in the step of the alkaline alcohol solution 4 of ko ko ko sodium hydroxide in alcoholic or alcoholic solution of ammonia.
  4. 4. ー种低明度和低红外发射率复合结构颜料的制备方法,包括以下步骤: 步骤I :采用粒径在I〜50微米的漂浮型片状铝粉,用无水こ醇将铝粉泡开并溶解其表面有机物,清洗、过滤、干燥后得到纯净的片状铝粉; 步骤2 :将Cr (NO3) 3 · 9H20溶于无水こ醇,控制Cr离子浓度在O. 03〜O. 2M之间; 步骤3 :将步骤I所得纯净的片状铝粉、步骤2所得Cr(NO3)3 ·9Η20的无水こ醇溶液和乳化剂0Ρ-10混合,控制混合体系中Cr (NO3) 3 ·9Η20与片状铝粉的摩尔比在(O. 04〜I. O) : I之间; 步骤4 :将步骤3所得混合体系置于40〜70°C环境下搅拌反应,搅拌反应过程中滴加碱性こ醇溶液,使混合体系PH值保持在7〜9之间;反应完毕后收集沉淀,并经清洗、干燥、研磨得到表面包覆Cr(OH)3的片状铝粉; 步骤5 :将步骤4所得表面包覆Cr (OH) 3的片状铝粉置于400〜450°C环境下煅烧处理,得到表面包覆纳米 4. The method of preparing low lightness and low infrared emissivity of the composite structure of the pigment ー species, comprising the following steps: Step I: floating aluminum flake particle employed in I~50 microns, with anhydrous aluminum blister ko ol dissolved organic matter and open surface thereof, washing, filtration, and dried to give pure aluminum flake; step 2: Cr (NO3) 3 · 9H20 dissolved in anhydrous alcohol ko, Cr ion concentration control O. 03~O. between 2M; step 3: step I obtained pure aluminum flake, step 2 resulting Cr (NO3) and an anhydrous alcohol solution of an emulsifier ko 3 · 9Η20 0Ρ-10 is mixed, the mixing control system Cr (NO3) the reaction was stirred for a mixed system obtained from step 3 was placed 40~70 ° C environment, stirred reaction:;: molar ratio of 3 · 9Η20 in the aluminum flakes (O. 04~I O.) step 4 between I ko alkaline alcohol solution was added dropwise, the combined system is held between the PH value 7~9; after completion of the reaction the precipitate is collected, washed and dried, dried, milled to obtain surface-coated Cr (OH) 3, aluminum flakes; step 5: the step of coating the surface 4 resulting Cr (OH) 3 was placed in aluminum flakes calcination treatment at 400~450 ° C environment, to obtain surface coated nano 化铬颗粒的片状铝粉,即低明度和低红外发射率的复合结构颜料。 Chromium aluminum flake particles, i.e., the composite structure of the pigment of low lightness and low infrared emissivity.
  5. 5.根据权利要求4所述的低明度和低红外发射率复合结构颜料的制备方法,其特征在于,在对步骤4所得表面包覆Cr (OH)3的片状铝粉进行步骤5所述煅烧处理之前,先对步骤4所得表面包覆Cr (OH) 3的片状铝粉进行水热处理,具体水热处理温度在150〜200°C之间,时间为4〜24小时。 The low brightness and a method for preparing the 4 low infrared emissivity of the composite structure of the pigment as claimed in claim wherein, in the step 5 of aluminum flakes coated surface obtained in step 4 Cr (OH) 3 is before calcination process, first coated Cr (OH) 3 aluminum flakes hydrothermal treatment obtained in step 4 of the surface, particularly the hydrothermal treatment at a temperature between 150~200 ° C, time of 4~24 hours.
  6. 6.根据权利要求I所述的低明度和低红外发射率复合结构颜料的制备方法,其特征在于,步骤4中所述碱性こ醇溶液为氢氧化钠的こ醇溶液或氨水的こ醇溶液。 I according to the method of preparing low lightness and low infrared emissivity of the composite structure of the pigment as claimed in claim wherein, in the step of the alkaline alcohol solution 4 of ko ko ko sodium hydroxide in alcoholic or aqueous ammonia alcohol solution.
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