Performance-adjustable iron oxide pigment and preparation method thereof

Abstract

The invention discloses a performance-adjustable iron oxide pigment and a preparation method thereof, and belongs to the technical field of inorganic pigment preparation. The iron oxide pigment comprises the following components: iron oxide, a doping material, triethanolamine, sulfonate sodium poly [(naphthaleneformaldehyde) sulfonate] and sodium silicate, wherein the doping material is zinc oxide, or copper oxide and nickel oxide, or zinc oxide and copper oxide. The iron oxide pigment prepared by the method is wide in hue range and has excellent tinting strength and saturation, the quality and use scene of the iron oxide pigment are improved, the preparation method is simple, the properties such as color, tinting strength and granularity are adjusted according to actual production requirements, and the iron oxide pigment is suitable for large-scale industrial production.

Description

Technical Field

[0001] The invention belongs to the technical field of inorganic pigment preparation, and particularly relates to an iron oxide pigment with adjustable performance and a preparation method thereof. Background Art

[0002] Iron oxide pigment is an environmentally friendly inorganic pigment. Its output is second only to titanium dioxide and it is currently the most widely used color pigment in the world. Iron oxide pigments mainly include three color systems: iron red (Fe2O3), iron yellow (FeOOH), and iron black (Fe3O4). These three colors are the most basic colors of artificially synthesized iron oxide. Mixing and compounding them together can form more than ten colors such as orange, brown, and green, showing a very complete color spectrum. Iron oxide pigments have stable physical and chemical properties, and have the advantages of alkali resistance, non-toxicity, light resistance, and low price. They are widely used in building materials, coatings, inks, rubber, plastics and other industries.

[0003] The iron content, water-soluble matter, pH value, sieve residue, moisture, oil absorption, tinting strength and color difference ΔE of iron oxide pigments are all quality indicators of iron oxide pigments. The quality indicators will directly affect its performance in various applications such as building materials and coatings. Color matching is one of the core technologies in the production of iron oxide red pigments. It is the selection, combination and uniform mixing of two or more produced iron oxide red pigments to obtain a color effect consistent with the target color. The color matching of iron oxide red pigments can obtain a uniform color because different colors of iron red are mixed and superimposed. The pigment particles themselves have size non-uniformity. The non-uniformity of particle size is equivalent to mixing different uniform iron oxide particles, which affects the final color and makes the color uneven and the hue inaccurate.

[0004] Therefore, it is necessary to provide an iron oxide pigment with adjustable properties. Summary of the invention

[0005] In view of the above problems existing in the prior art, the first technical problem to be solved by the present invention is to provide an iron oxide pigment with adjustable performance, which has a wide range of hues and excellent tinting strength and saturation. The second technical problem to be solved by the present invention is to provide a method for preparing an iron oxide pigment with adjustable performance, which is simple and convenient, and the prepared iron oxide pigment has a wide range of hues.

[0006] In order to solve the above problems, the technical solution adopted by the present invention is as follows:

[0007] A performance-adjustable iron oxide pigment comprises components of iron oxide, doping materials, triethanolamine, sulfonate polynaphthaldehyde sulfonate sodium salt and sodium silicate; wherein the doping materials are zinc oxide, or copper oxide and nickel oxide, or zinc oxide and copper oxide.

[0008] Furthermore, when the doping material is zinc oxide, the mass ratio of iron oxide to zinc oxide is 4:1.

[0009] Furthermore, when the doping materials are copper oxide and nickel oxide, the mass ratio of iron oxide, copper oxide and nickel oxide is 7:2:1.

[0010] Furthermore, when the doping materials are zinc oxide and copper oxide, the mass ratio of iron oxide, zinc oxide and copper oxide is 6:3:1.

[0011] Furthermore, the mass of the triethanolamine is 0.02% to 0.05% of the total mass of the iron oxide and the doping material.

[0012] Furthermore, the mass of the sulfonate polynaphthaldehyde sulfonate sodium salt is 0.1% to 0.2% of the total mass of the iron oxide and the doping material.

[0013] Furthermore, the mass of the sodium silicate is 1% to 1.5% of the total mass of the iron oxide and the doping material.

[0014] A method for preparing an iron oxide pigment with adjustable performance comprises the following steps: firstly dissolving sodium silicate in water at 50-55°C for 2-2.5 hours to prepare a sodium silicate aqueous solution; then mixing iron oxide, a doping material, triethanolamine and sulfonate polynaphthaldehyde sulfonate sodium salt with the sodium silicate aqueous solution, stirring evenly, drying and calcining to obtain the iron oxide pigment.

[0015] Furthermore, the drying temperature is 150-160°C.

[0016] Furthermore, the calcination temperature is 750-900°C.

[0017] Beneficial effects: Compared with the prior art, the advantages of the present invention are:

[0018] (1) The iron oxide pigment prepared by the present invention has a wide hue range and excellent tinting strength and saturation, which increases the quality and application scenarios of the iron oxide pigment.

[0019] (2) The performance of the iron oxide pigment prepared by the present invention is adjustable. The color, tinting strength and particle size of the iron oxide pigment prepared by changing the ratio of raw materials according to actual production conditions are adjustable, and the application range is wide.

[0020] (3) The preparation method of the present invention is simple, the raw material cost is low, and it can be used for large-scale industrial production. DETAILED DESCRIPTION

[0021] The present invention is further described below in conjunction with specific embodiments.

[0022] Example 1

[0023] The preparation method of iron oxide pigment is as follows:

[0024] First, sodium silicate is dissolved in water at 55°C for 2 hours to prepare a sodium silicate aqueous solution; then iron oxide, zinc oxide, triethanolamine and sodium polynaphthaldehyde sulfonate are mixed with the sodium silicate aqueous solution, stirred evenly, dried at 150°C, and then calcined at 800°C to obtain an iron oxide pigment. Among them, the mass ratio of iron oxide to zinc oxide is 4:1, the mass of triethanolamine is 0.02% of the total mass of iron oxide and zinc oxide, the mass of sodium polynaphthaldehyde sulfonate is 0.1% of the total mass of iron oxide and zinc oxide, and the mass of sodium silicate is 1% of the total mass of iron oxide and zinc oxide.

[0025] Example 2

[0026] The preparation method of iron oxide pigment is as follows:

[0027] First, sodium silicate is dissolved in water at 55°C for 2 hours to prepare a sodium silicate aqueous solution; then iron oxide, zinc oxide, triethanolamine and sodium polynaphthaldehyde sulfonate are mixed with the sodium silicate aqueous solution, stirred evenly, dried at 150°C, and then calcined at 800°C to obtain an iron oxide pigment. Among them, the mass ratio of iron oxide to zinc oxide is 4:1, the mass of triethanolamine is 0.04% of the total mass of iron oxide and zinc oxide, the mass of sodium polynaphthaldehyde sulfonate is 0.1% of the total mass of iron oxide and zinc oxide, and the mass of sodium silicate is 1% of the total mass of iron oxide and zinc oxide.

[0028] Example 3

[0029] The preparation method of iron oxide pigment is as follows:

[0030] First, sodium silicate is dissolved in water at 55°C for 2 hours to prepare a sodium silicate aqueous solution; then iron oxide, zinc oxide, triethanolamine and sodium polynaphthaldehyde sulfonate are mixed with the sodium silicate aqueous solution, stirred evenly, dried at 150°C, and then calcined at 800°C to obtain an iron oxide pigment. Among them, the mass ratio of iron oxide to zinc oxide is 4:1, the mass of triethanolamine is 0.05% of the total mass of iron oxide and zinc oxide, the mass of sodium polynaphthaldehyde sulfonate is 0.1% of the total mass of iron oxide and zinc oxide, and the mass of sodium silicate is 1% of the total mass of iron oxide and zinc oxide.

[0031] Example 4

[0032] The preparation method of iron oxide pigment is as follows:

[0033] First, sodium silicate is dissolved in water at 55°C for 2 hours to prepare a sodium silicate aqueous solution; then iron oxide, copper oxide, nickel oxide, triethanolamine and sulfonate polynaphthaldehyde sulfonate sodium salt are mixed with the sodium silicate aqueous solution, stirred evenly, dried at 150°C, and then calcined at 800°C to obtain an iron oxide pigment. Among them, the mass ratio of iron oxide, copper oxide and nickel oxide is 7:2:1, the mass of triethanolamine is 0.05% of the total mass of iron oxide and zinc oxide, the mass of sulfonate polynaphthaldehyde sulfonate sodium salt is 0.1% of the total mass of iron oxide and zinc oxide, and the mass of sodium silicate is 1% of the total mass of iron oxide and zinc oxide.

[0034] Example 5

[0035] First, sodium silicate is dissolved in water at 55°C for 2 hours to prepare a sodium silicate aqueous solution; then iron oxide, copper oxide, nickel oxide, triethanolamine and sodium sulfonate polynaphthaldehyde sulfonate are mixed with the sodium silicate aqueous solution, stirred evenly, dried at 150°C, and then calcined at 800°C to obtain an iron oxide pigment. Among them, the mass ratio of iron oxide, copper oxide and nickel oxide is 7:2:1, the mass of triethanolamine is 0.05% of the total mass of iron oxide and zinc oxide, the mass of sodium sulfonate polynaphthaldehyde sulfonate is 0.1% of the total mass of iron oxide and zinc oxide, and the mass of sodium silicate is 1.5% of the total mass of iron oxide and zinc oxide.

[0036] Example 6

[0037] The preparation method of iron oxide pigment is as follows:

[0038] First, sodium silicate is dissolved in water at 55°C for 2 hours to prepare a sodium silicate aqueous solution; then iron oxide, zinc oxide, copper oxide, triethanolamine and sulfonate polynaphthaldehyde sulfonate sodium salt are mixed with the sodium silicate aqueous solution, stirred evenly, dried at 150°C, and then calcined at 800°C to obtain an iron oxide pigment. Among them, the mass ratio of iron oxide, zinc oxide and copper oxide is 6:3:1, the mass of triethanolamine is 0.05% of the total mass of iron oxide and zinc oxide, the mass of sulfonate polynaphthaldehyde sulfonate sodium salt is 0.1% of the total mass of iron oxide and zinc oxide, and the mass of sodium silicate is 1% of the total mass of iron oxide and zinc oxide.

[0039] Example 7

[0040] The preparation method of iron oxide pigment is as follows:

[0041] First, sodium silicate is dissolved in water at 55°C for 2 hours to prepare a sodium silicate aqueous solution; then iron oxide, zinc oxide, copper oxide, triethanolamine and sulfonate polynaphthaldehyde sulfonate sodium salt are mixed with the sodium silicate aqueous solution, stirred evenly, dried at 150°C, and then calcined at 800°C to obtain an iron oxide pigment. Among them, the mass ratio of iron oxide, zinc oxide and copper oxide is 6:3:1, the mass of triethanolamine is 0.05% of the total mass of iron oxide and zinc oxide, the mass of sulfonate polynaphthaldehyde sulfonate sodium salt is 0.1% of the total mass of iron oxide and zinc oxide, and the mass of sodium silicate is 1.5% of the total mass of iron oxide and zinc oxide.

[0042] Example 8

[0043] 1. After the iron oxide pigments prepared in Examples 1 to 7 were placed in a constant temperature and humidity chamber for 72 hours, the results are shown in Table 1 below.

[0044] Table 1 Stability results of iron oxide pigments prepared in Examples 1 to 7

[0045]

[0046]

[0047] Table 1 shows the stability results of the iron oxide pigments prepared in Examples 1 to 7 of the present invention. It can be seen from the table that after being in a constant temperature and humidity chamber for 72 hours, the mass of the iron oxide pigments prepared by the present invention changes little, and the color does not change significantly, proving that the iron oxide pigments prepared by the present invention are stable and excellent.

[0048] 2. Tinting strength test

[0049] The tinting strength of the iron oxide pigments prepared in Examples 1 to 7 was measured using a colorimeter in accordance with the provisions of GB / T13451.2. The results are shown in Table 2 below.

[0050] Table 2 Tinting strength test of iron oxide pigments prepared in Examples 1 to 7

[0051]

[0052] Table 2 is the tinting power test of the iron oxide pigments prepared in Examples 1 to 7. It can be seen from the table that the iron oxide pigments prepared in the present invention all have excellent tinting power.

[0053] 3. Color difference analysis

[0054] The iron oxide red prepared in Examples 1 to 7 was measured using a spectrophotometer (CM-5 model of Minolta Company) and a pigment color development test method. 0.1 g of iron oxide pigment and 1 g of zinc oxide were weighed, mixed evenly with 0.8 mL of varnish, and a thin layer of color paste was applied on a glass sheet. The color was then measured and analyzed using a color measurement software to obtain the ΔL, Δa, and Δb values ​​(hue) of the iron oxide red sample color, which were expressed by the following expression:

[0055] ΔL=L-L0

[0056] Δa=a-a0

[0057] Δb=b-b0

[0058] Among them, L, a, b are lightness, red-green value and yellow-blue value respectively, and L0, a0, b0 are the color values ​​of the standard sample.

[0059] Finally, it was concluded that ΔL, Δa, and Δb were all within ±0.25, indicating that the iron oxide red pigment prepared by the present invention has small color difference change, is stable, and has good quality.

[0060] 4. Particle size test

[0061] The particle size of the iron oxide pigments prepared in Examples 1 to 7 was measured using a laser particle size analyzer. The results are shown in Table 3 below.

[0062] Table 3 Particle size analysis results of iron oxide pigments prepared in Examples 1 to 7

[0063] <![CDATA[D 10 (μm)]]> <![CDATA[D 50 (μm)]]> <![CDATA[D 90 (μm)]]> Example 1 0.24 0.52 1.47 Example 2 0.24 0.54 1.42 Example 3 0.26 0.52 1.42 Example 4 0.31 0.49 1.43 Example 5 0.28 0.48 1.59 Example 6 0.24 0.43 1.56 Example 7 0.23 0.54 1.53 Example 8 0.24 0.51 1.42

[0064] Table 3 is the particle size analysis results of the iron oxide pigments prepared in Examples 1 to 7. It can be seen from the table that the iron oxide pigments prepared by the present invention have a narrow particle size distribution, more uniform particles, excellent tinting power, and good dispersibility, fluidity and weather resistance.

Claims

1. A performance-adjustable iron oxide pigment, characterized in that: The components of the iron oxide pigment include iron oxide, doping material, triethanolamine, sulfonate polynaphthaldehyde sulfonate sodium salt and sodium silicate; wherein the doping material is zinc oxide, or copper oxide and nickel oxide, or zinc oxide and copper oxide.

2. The performance-adjustable iron oxide pigment according to claim 1, characterized in that: When the doping material is zinc oxide, the mass ratio of iron oxide to zinc oxide is 4:

1.

3. The performance-adjustable iron oxide pigment according to claim 1, characterized in that: When the doping materials are copper oxide and nickel oxide, the mass ratio of iron oxide, copper oxide and nickel oxide is 7:2:

1.

4. The performance-adjustable iron oxide pigment according to claim 1, characterized in that: When the doping materials are zinc oxide and copper oxide, the mass ratio of iron oxide, zinc oxide and copper oxide is 6:3:

1.

5. The performance-adjustable iron oxide pigment according to claim 1, characterized in that: The mass of the triethanolamine is 0.02% to 0.05% of the total mass of the iron oxide and the doping material.

6. The performance-adjustable iron oxide pigment according to claim 1, characterized in that: The mass of the sulfonate polynaphthaldehyde sulfonate sodium salt is 0.1% to 0.2% of the total mass of the iron oxide and the doping material.

7. The performance-adjustable iron oxide pigment according to claim 1, characterized in that: The mass of the sodium silicate is 1% to 1.5% of the total mass of the iron oxide and the doping material.

8. A method for preparing an iron oxide pigment with adjustable properties, characterized in that: Firstly, sodium silicate is dissolved in water at 50-55°C for 2-2.5 hours to prepare a sodium silicate aqueous solution; then, iron oxide, doping material, triethanolamine and sulfonate polynaphthaldehyde sulfonate sodium salt are mixed with the sodium silicate aqueous solution, stirred evenly, dried and calcined to obtain an iron oxide pigment.

9. The method for preparing the performance-adjustable iron oxide pigment according to claim 8, characterized in that: The drying temperature is 150-160°C.

10. The method for preparing the performance-adjustable iron oxide pigment according to claim 8, characterized in that: The calcination temperature is 750-900°C.

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