WO2023201973A1 - Synthesis method for wide-chromatographic-band iron oxide yellow pigment - Google Patents
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000001052 yellow pigment Substances 0.000 title claims abstract description 9
- 238000001308 synthesis method Methods 0.000 title description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 21
- HNJXPTMEWIVQQM-UHFFFAOYSA-M triethyl(hexadecyl)azanium;bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](CC)(CC)CC HNJXPTMEWIVQQM-UHFFFAOYSA-M 0.000 claims description 6
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 abstract description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 abstract description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 abstract description 6
- 239000004809 Teflon Substances 0.000 abstract description 4
- 229920006362 Teflon® Polymers 0.000 abstract description 4
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 4
- 239000010935 stainless steel Substances 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 238000005303 weighing Methods 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 230000008569 process Effects 0.000 description 8
- 229910002588 FeOOH Inorganic materials 0.000 description 6
- 239000000049 pigment Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000001034 iron oxide pigment Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 239000001023 inorganic pigment Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000009965 odorless effect Effects 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012812 general test Methods 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- 229910006540 α-FeOOH Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide (Fe2O3)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/22—Compounds of iron
- C09C1/24—Oxides of iron
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- Compounds Of Iron (AREA)
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Abstract
A preparation method for a wide-chromatographic-band iron oxide yellow pigment. The preparation method comprises: 1, weighing 0.03-0.08 mol of CTAB (hexadecyl trimethyl ammonium bromide), dispersing in 30-50 mL of deionized water, stirring at room temperature for 30-60 min until a solution becomes transparent, and denoting the solution as a solution A; 2, separately weighing 0.02-0.2 mol of FeCl3 (ferric chloride), dissolving the FeCl3 in the solution A, and stirring for 30-60 min until a homogeneous solution is formed; 3, pouring the solution into a 50 mL Teflon stainless steel high-pressure reaction kettle and carrying out a hydrothermal reaction at 80-120 °C for 6-24 h; 4, after the reaction is completed, cooling the reaction kettle to room temperature; and 5, separately washing with ethanol and distilled water three times and drying at 50-60°. Finally, the wide-chromatographic-band iron oxide yellow with ΔL reaching 5.17 and ΔB reaching 7.18 is obtained.
Description
本发明涉及颜料领域，特别涉及具有宽色谱带的氧化铁黄颜料的制备方法。The present invention relates to the field of pigments, and in particular to a method for preparing iron oxide yellow pigments with wide chromatographic bands.
氧化铁颜料是传统的着色无机颜料，是仅次于钛白粉的世界上第二大无机颜料，也是第一大彩色无机颜料。氧化铁颜料分散性好,防腐蚀性佳,成本低廉,现广泛应用于各种户外用漆、交通用漆、金属防锈用底漆及面漆中。氧化铁能用于玻璃制品及玻璃五金抛光中。氧化铁分子颗粒细而均匀,比表面积大,因而可应用于化学触媒上。氧化铁颜料性能稳定,无毒、无嗅、无味、人体不吸收、无副作用、无油渗性、不损害皮肤,颜色久晒不变,可长久保存。因此,氧化铁颜料在食品、医药、化妆品及化妆油彩着色上得到广泛应用。Iron oxide pigment is a traditional colored inorganic pigment. It is the second largest inorganic pigment in the world after titanium dioxide and the largest colored inorganic pigment. Iron oxide pigments have good dispersion, good anti-corrosion properties and low cost. They are now widely used in various outdoor paints, traffic paints, and metal anti-rust primers and topcoats. Iron oxide can be used in polishing glass products and glass hardware. Iron oxide molecules have fine and uniform particles and a large specific surface area, so they can be used as chemical catalysts. Iron oxide pigments have stable performance, are non-toxic, odorless, tasteless, non-absorbable by the human body, have no side effects, have no oil permeability, do not damage the skin, the color will not change after being exposed to the sun for a long time, and can be stored for a long time. Therefore, iron oxide pigments are widely used in food, medicine, cosmetics and cosmetic oil coloring.
氧化铁黄(又称羟基氧化铁)的化学式为α-Fe
2O
3·H
2O或α-FeOOH，呈针状或棒状结构，通常短轴径小于0.1μm，长轴径在0.6μm左右，外观为黄色粉末状，在透明介质中有很好分散性的铁系颜料，其着色力强，遮盖力高，不溶于碱，微溶于酸。氧化铁黄具有耐光性、分散性好以及无毒、无味，人体不易吸收等特点，广泛应用于涂料、塑料、油墨以及医药工业等领域
The chemical formula of iron oxide yellow (also known as iron oxyhydroxide) is α-Fe 2 O 3 ·H 2 O or α-FeOOH. It has a needle-like or rod-like structure. Usually the short axis diameter is less than 0.1 μm and the long axis diameter is about 0.6 μm. , an iron-based pigment with a yellow powder appearance and good dispersion in transparent media. It has strong tinting power and high hiding power. It is insoluble in alkali and slightly soluble in acid. Iron oxide yellow has the characteristics of light resistance, good dispersion, non-toxic, odorless, and not easily absorbed by the human body. It is widely used in coatings, plastics, inks, pharmaceutical industries and other fields.
目前常见的铁黄颜料通常呈针状，研究表明长径比影响其颜色这个最为关键的性能，但是实验表明，长径比越长，颜色向黄相转换；长径比越短，颜色向红相转变。常见的氧化铁黄由于有效工艺范围内对晶型尺寸的控制较小，如业内普遍采用氧化时间的控制来改变氧化铁黄的长轴尺寸，以得到不同色相的氧化铁黄，但是该工艺所能控制氧化铁黄B值和L值的范围很小，通过钛白粉冲淡试验△L值、△B的变化范围仅在3.00范围内。因此，该工艺所能得到的氧化铁黄的品种太少，无法满足各行各业对不同氧化铁黄色相的要求，因此，我们对本专利技术进行研究，希望能够研发出更宽色谱变化的氧化铁黄制备工艺。Currently common iron yellow pigments are usually needle-shaped. Research shows that the aspect ratio affects the most critical performance of its color. However, experiments show that the longer the aspect ratio, the color changes to yellow; the shorter the aspect ratio, the color turns to red. phase transition. Common iron oxide yellow has little control over the crystal size within the effective process range. For example, the industry generally uses control of oxidation time to change the long axis size of iron oxide yellow to obtain iron oxide yellow with different hues. However, this process requires The range that can control the B value and L value of iron oxide yellow is very small. Through the titanium dioxide dilution test, the variation range of △L value and △B is only within the range of 3.00. Therefore, there are too few varieties of iron oxide yellow that can be obtained by this process, which cannot meet the requirements of various industries for different yellow phases of iron oxide. Therefore, we conduct research on this patented technology in the hope of developing iron oxide with wider chromatographic changes. Yellow preparation process.
发明内容Contents of the invention
本发明所要解决的技术问题在于提供一种通过控制氧化铁黄长径比提高氧化铁黄色谱宽度的合成方法。The technical problem to be solved by the present invention is to provide a synthesis method for increasing the spectrum width of iron oxide yellow by controlling the aspect ratio of iron oxide yellow.
为了实现上述的目的，本发明采用了以下的技术方案：In order to achieve the above objects, the present invention adopts the following technical solutions:
一种宽色谱带氧化铁黄颜料的合成方法，该方法包括如下步骤：A method for synthesizing iron oxide yellow pigment with a wide chromatographic band, the method includes the following steps:
步骤1)称取十六烷基三乙基溴化铵分散于去离子水中，室温下搅拌直至溶液变得透明，记为溶液A；Step 1) Weigh cetyltriethylammonium bromide and disperse it in deionized water, stir at room temperature until the solution becomes transparent, and record it as solution A;
步骤2)称取FeCl
3溶于溶液A中，搅拌直至形成均相溶液，其中，所述的所述十六烷 基三乙基溴化铵、FeCl
3与去离子水比例为0.03～0.08mol：0.02mol～0.2mol：30～50mL；
Step 2) Weigh FeCl 3 and dissolve it in solution A, stir until a homogeneous solution is formed, wherein the ratio of cetyl triethylammonium bromide, FeCl 3 and deionized water is 0.03 to 0.08 mol ：0.02mol～0.2mol：30～50mL;
步骤3)将溶液倒入高压反应釜中，在80～120℃下水热6～24h；Step 3) Pour the solution into a high-pressure reaction kettle and heat it with water at 80-120°C for 6-24 hours;
步骤4)反应结束后，反应釜冷却至室温；Step 4) After the reaction is completed, the reaction kettle is cooled to room temperature;
步骤5)用乙醇和蒸馏水分别洗涤，烘干干燥。Step 5) Wash with ethanol and distilled water respectively, and dry by drying.
在一些具体实施例中，该方法包括如下步骤：In some specific embodiments, the method includes the following steps:
步骤1)称取0.03～0.08mol十六烷基三乙基溴化铵分散于30～50mL去离子水中，室温下搅拌30-60min直至溶液变得透明，记为溶液A；Step 1) Weigh 0.03 to 0.08 mol of cetyltriethylammonium bromide and disperse it in 30 to 50 mL of deionized water. Stir at room temperature for 30 to 60 minutes until the solution becomes transparent, which is recorded as solution A;
步骤2)称取0.02mol～0.2mol的FeCl
3溶于溶液A中，搅拌30～60min直至形成均相溶液；
Step 2) Weigh 0.02 mol ~ 0.2 mol FeCl 3 and dissolve it in solution A, stir for 30 ~ 60 minutes until a homogeneous solution is formed;
步骤3)将溶液倒入高压反应釜中，在80～120℃下水热6～24h；Step 3) Pour the solution into a high-pressure reaction kettle and heat it with water at 80-120°C for 6-24 hours;
步骤4)反应结束后，反应釜冷却至室温；Step 4) After the reaction is completed, the reaction kettle is cooled to room temperature;
步骤5)用乙醇和蒸馏水分别洗涤3次，50～60℃下烘干干燥。Step 5) Wash 3 times with ethanol and distilled water respectively, and dry at 50-60°C.
本发明在制备氧化铁黄颜料的过程中加入十六烷基三甲基溴化铵(CTAB)，CTAB溶解在水中时会产生CTA
+，它可以充当软模板并防止聚集。在氧化铁黄颜料的合成过程中，CTAB的存在控制了颗粒之间的相互作用，从而降低了微晶尺寸；CTAB作为阳离子表面活性剂，在溶液中产生CTA
+，可吸附在颗粒表面。随着FeCl
3浓度增加，带电离子之间的排斥阻止了聚集，产生了尺寸更小的FeOOH颗粒，因此通过控制FeCl
3浓度可以控制FeOOH的长径比。
In the present invention, cetyltrimethylammonium bromide (CTAB) is added in the process of preparing iron oxide yellow pigment. When CTAB is dissolved in water, CTA + will be produced, which can act as a soft template and prevent aggregation. During the synthesis process of iron oxide yellow pigment, the presence of CTAB controls the interaction between particles, thereby reducing the crystallite size; CTAB, as a cationic surfactant, produces CTA + in the solution and can be adsorbed on the particle surface. As the FeCl concentration increases, the repulsion between charged ions prevents aggregation and produces FeOOH particles with smaller sizes, so the aspect ratio of FeOOH can be controlled by controlling the FeCl concentration.
与现有技术相比，本发明具有如下技术效果：Compared with the existing technology, the present invention has the following technical effects:
1.本发明提供的合成方法简单，能够得到晶型优良的棒状FeOOH；1. The synthesis method provided by the present invention is simple and can obtain rod-shaped FeOOH with excellent crystal form;
2.采用本发明的合成方法，可以制备出不同长径比的棒状羟基氧化铁。2. Using the synthesis method of the present invention, rod-shaped iron oxyhydroxides with different aspect ratios can be prepared.
图1为实施例1，2，3的XRD图；Figure 1 is the XRD pattern of Examples 1, 2, and 3;
图2为实施例1中的SEM图；Figure 2 is a SEM image in Example 1;
图3为实施例2中的SEM图；Figure 3 is an SEM image in Example 2;
图4为实施例3中的SEM图。Figure 4 is an SEM image in Example 3.
下面通过具体的实验对本发明作进一步的说明：The present invention will be further explained below through specific experiments:
实施例1 FeOOH长径比为4-样品1Example 1 FeOOH aspect ratio is 4 - sample 1
1)称取0.04mol CTAB(十六烷基三甲基溴化铵)分散于50mL去离子水中，室温下搅拌30min直至溶液变得透明，记为溶液A；1) Weigh 0.04 mol CTAB (cetyltrimethylammonium bromide) and disperse it in 50 mL deionized water. Stir at room temperature for 30 minutes until the solution becomes transparent, recorded as solution A;
2)分别称取0.03mol的FeCl
3(氯化铁)溶于溶液A中，搅拌30-60min直至形成均相 溶液；
2) Weigh 0.03 mol of FeCl 3 (ferric chloride) and dissolve in solution A, stir for 30-60 minutes until a homogeneous solution is formed;
3)将溶液倒入50mL Teflon的不锈钢高压反应釜中，在120℃下水热12h；3) Pour the solution into a 50mL Teflon stainless steel high-pressure reactor and heat it with water at 120°C for 12 hours;
4)反应结束后，反应釜冷却至室温。4) After the reaction is completed, the reaction kettle is cooled to room temperature.
5)用乙醇和蒸馏水分别洗涤3次，60℃下烘干干燥。5) Wash 3 times with ethanol and distilled water respectively, and dry at 60°C.
实施例2 FeOOH长径比为5-样品2Example 2 FeOOH aspect ratio is 5 - sample 2
1)称取0.04mol CTAB(十六烷基三甲基溴化铵)分散于50mL去离子水中，室温下搅拌30min直至溶液变得透明，记为溶液A；1) Weigh 0.04 mol CTAB (cetyltrimethylammonium bromide) and disperse it in 50 mL deionized water. Stir at room temperature for 30 minutes until the solution becomes transparent, recorded as solution A;
2)分别称取0.04mol的FeCl
3(氯化铁)溶于溶液A中，搅拌30-60min直至形成均相溶液；
2) Weigh 0.04 mol of FeCl 3 (ferric chloride) and dissolve it in solution A, stir for 30-60 minutes until a homogeneous solution is formed;
3)将溶液倒入50mL Teflon的不锈钢高压反应釜中，在120℃下水热12h；3) Pour the solution into a 50mL Teflon stainless steel high-pressure reactor and heat it with water at 120°C for 12 hours;
4)反应结束后，反应釜冷却至室温。4) After the reaction is completed, the reaction kettle is cooled to room temperature.
5)用乙醇和蒸馏水分别洗涤3次，60℃下烘干干燥。5) Wash 3 times with ethanol and distilled water respectively, and dry at 60°C.
实施例3 FeOOH长径比为7-样品3Example 3 FeOOH aspect ratio is 7 - sample 3
1)称取0.04mol CTAB(十六烷基三甲基溴化铵)分散于50mL去离子水中，室温下搅拌30min直至溶液变得透明，记为溶液A；1) Weigh 0.04 mol CTAB (cetyltrimethylammonium bromide) and disperse it in 50 mL deionized water. Stir at room temperature for 30 minutes until the solution becomes transparent, recorded as solution A;
2)分别称取0.08mol的FeCl
3(氯化铁)溶于溶液A中，搅拌30-60min直至形成均相溶液；
2) Weigh 0.08 mol of FeCl 3 (ferric chloride) and dissolve in solution A, stir for 30-60 minutes until a homogeneous solution is formed;
3)将溶液倒入50mL Teflon的不锈钢高压反应釜中，在120℃下水热12h；3) Pour the solution into a 50mL Teflon stainless steel high-pressure reactor and heat it with water at 120°C for 12 hours;
4)反应结束后，反应釜冷却至室温。4) After the reaction is completed, the reaction kettle is cooled to room temperature.
5)用乙醇和蒸馏水分别洗涤3次，60℃下烘干干燥。5) Wash 3 times with ethanol and distilled water respectively, and dry at 60°C.
通过实施例1-3的三组实验获得产品进行XRD与SEM测试，测试结果如图1与表1所示。The products obtained through the three sets of experiments in Examples 1-3 were subjected to XRD and SEM tests. The test results are shown in Figure 1 and Table 1.
根据GB/T 1864-2012颜料和体制颜料通用试验方法颜料颜色的比较的规定进行研磨，再利用测色仪进行颜色测定，具体数据如下表1：Grind according to the provisions of GB/T 1864-2012 Comparison of Pigment Colors in General Test Methods for Pigments and Institutional Pigments, and then use a colorimeter to measure the color. The specific data are as follows in Table 1:
表1Table 1
通过3组实验可以明显看出，其长径比得到了显著的变化，可达到1：4-1：12，L值的变化值域范围达到5.17，B值的值域范围达到7.18，特别是该工艺的B值达到49.35，色彩饱和度远高于普通工艺的44.82。(普通工艺的长径比只能控制在1：5-1：8，L值和B值均在3.0以内，B值仅能达到44.82，饱和度较差)也就是说通过专利方案调整长径比后色谱范围明显变宽，更加能够满足不同应用领域对氧化铁黄色相的要求。Through three sets of experiments, it can be clearly seen that the aspect ratio has changed significantly, reaching 1:4-1:12, the change range of the L value has reached 5.17, and the range of the B value has reached 7.18, especially The B value of this process reaches 49.35, and the color saturation is much higher than the 44.82 of the ordinary process. (The aspect ratio of ordinary processes can only be controlled at 1:5-1:8, the L value and B value are both within 3.0, the B value can only reach 44.82, and the saturation is poor) In other words, the length diameter is adjusted through a patented solution Compared with the latter, the chromatographic range is significantly wider, which can better meet the requirements for the yellow phase of iron oxide in different application fields.
Claims (5)
- 一种宽色谱带氧化铁黄颜料的合成方法，其特征在于，该方法包括如下步骤：A method for synthesizing iron oxide yellow pigment with a wide chromatographic band, which is characterized in that the method includes the following steps:步骤1)称取十六烷基三乙基溴化铵分散于去离子水中，室温下搅拌直至溶液变得透明，记为溶液A；Step 1) Weigh cetyltriethylammonium bromide and disperse it in deionized water, stir at room temperature until the solution becomes transparent, and record it as solution A;步骤2)称取FeCl 3溶于溶液A中，搅拌直至形成均相溶液，其中，所述的所述十六烷基三乙基溴化铵、FeCl 3与去离子水比例为0.03～0.08mol：0.02mol～0.2mol：30～50mL； Step 2) Weigh FeCl 3 and dissolve it in solution A, stir until a homogeneous solution is formed, wherein the ratio of cetyl triethylammonium bromide, FeCl 3 and deionized water is 0.03 to 0.08 mol ：0.02mol～0.2mol：30～50mL;步骤3)将溶液倒入高压反应釜中，在80～120℃下水热6～24h；Step 3) Pour the solution into a high-pressure reaction kettle and heat it with water at 80-120°C for 6-24 hours;步骤4)反应结束后，反应釜冷却至室温；Step 4) After the reaction is completed, the reaction kettle is cooled to room temperature;步骤5)用乙醇和蒸馏水分别洗涤，烘干干燥。Step 5) Wash with ethanol and distilled water respectively, and dry by drying.
- 如权利要求1所述的方法，其特征在于，步骤(1)中搅拌时间控制在30-60min之间。The method according to claim 1, characterized in that in step (1), the stirring time is controlled between 30-60 minutes.
- 如权利要求1所述的方法，其特征在于，步骤5)用乙醇和蒸馏水分别洗涤3次，50～60℃下烘干干燥The method according to claim 1, characterized in that step 5) is washed three times with ethanol and distilled water respectively, and dried at 50-60°C.
- 如权利要求1所述的方法，其特征在于，该方法包括如下步骤：The method according to claim 1, characterized in that the method includes the following steps:步骤1)称取0.03～0.08mol十六烷基三乙基溴化铵分散于30～50mL去离子水中，室温下搅拌30-60min直至溶液变得透明，记为溶液A；Step 1) Weigh 0.03 to 0.08 mol of cetyltriethylammonium bromide and disperse it in 30 to 50 mL of deionized water. Stir at room temperature for 30 to 60 minutes until the solution becomes transparent, which is recorded as solution A;步骤2)称取0.02mol～0.2mol的FeCl 3溶于溶液A中，搅拌30～60min直至形成均相溶液； Step 2) Weigh 0.02 mol ~ 0.2 mol FeCl 3 and dissolve it in solution A, stir for 30 ~ 60 minutes until a homogeneous solution is formed;步骤3)将溶液倒入高压反应釜中，在80～120℃下水热6～24h；Step 3) Pour the solution into a high-pressure reaction kettle and heat it with water at 80-120°C for 6-24 hours;步骤4)反应结束后，反应釜冷却至室温；Step 4) After the reaction is completed, the reaction kettle is cooled to room temperature;步骤5)用乙醇和蒸馏水分别洗涤3次，50～60℃下烘干干燥。Step 5) Wash 3 times with ethanol and distilled water respectively, and dry at 50-60°C.
- 如权利要求1～4任意一项所述的方法获得的氧化铁黄颜料。The iron oxide yellow pigment obtained by the method according to any one of claims 1 to 4.
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