Method for mechanochemical preparation of high-performance iron red/clay mineral hybrid pigment

Abstract

The disclosure relates to a method for mechanochemical preparation of an iron red pigment, which comprise steps: mixing a clay mineral, a soluble iron source and an alkali source in a mill for grinding to obtain a precursor, wherein the ratio of ball to material is controlled at 20-50, the grinding speed is 300-1200 rpm, and the grinding time is 30-360 min; and calcining the precursor at 500-900° C. for 30-120 min to obtain a high-performance iron oxide red/clay mineral hybrid pigment. The iron oxide red/clay mineral hybrid pigment has a bright and beautiful color, high-temperature and acid resistance, and can satisfy requirements for high-performance iron oxide red pigments in fields of paints, inks, ceramics, anti-corrosive coatings, etc. Furthermore the method is a simple process without waste that is environmentally friendly and suitable for industrialized production, thus it is expected to replace existing processes of iron oxide red pigments.

Claims

1. A method for mechanochemical preparation of an iron red/clay mineral hybrid pigment, comprising the flowing steps: adding a mixture composed of clay minerals, soluble iron sources and alkali sources into a planetary ball mill for grinding to obtain a precursor, and then calcining the obtained precursor at a temperature to obtain the iron red/clay mineral hybrid pigment, wherein an amount of the soluble iron source is 0.5-4 times of the amount of the clay minerals, wherein an amount of the alkali source is 0.2-2.0 times of the amount of the soluble iron source, wherein an amount ratio of ball to the mixture is 20-50, a grinding speed is 300-1200 rpm, and a grinding time is 60-360 minutes during grinding, and wherein the calcination temperature of the precursor is 500-900° C., and a calcination time is 30-120 minutes.

2. The method for mechanochemical preparation of the iron red/clay mineral hybrid pigment according to claim 1, wherein the clay minerals are acids and heat treated natural clay minerals.

3. The method for mechanochemical preparation the iron red/clay mineral hybrid pigment according to claim 1, wherein the clay minerals are selected from the group consisting of attapulgite, montmorillonite, kaolinite, halloysite, sepiolite, serpentine, mica, vermiculite, and rectorite.

4. The method for mechanochemical preparation of the iron red/clay mineral hybrid pigment according to claim 1, wherein the soluble iron sources are at least one of ferric chloride, ferric sulfate, ferric nitrate, ferrous chloride, ferrous sulfate, ferrous acetate, and ferrous nitrate.

5. The method for mechanochemical preparation of iron red/clay mineral hybrid pigments according to claim 1, wherein the alkali sources are at least one of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, sodium phosphate, and disodium phosphate.

Description

BRIEF DESCRIPTION OF DRAWINGS

(1) The sole FIGURE is the X-ray diffraction patterns of the iron red/clay mineral hybrid pigment prepared by the present disclosure.

DETAILED DESCRIPTION

(2) The preparation and performance of the high-performance iron red/clay mineral hybrid pigment of the present disclosure will be further illustrated by specific Examples below.

Example 1

(3) 0.25 g of attapulgite, 0.127 g of ferric chloride and 0.050 g of sodium hydroxide were mixed and put into a 45 mL zirconium dioxide ball mill. 17.31 g of 2 mm zirconium dioxide balls with a ball to material ratio of 20 was added and ground at 400 rpm for 120 min, and the obtained precursor was calcined at 700° C. for 60 min. The obtained iron red hybrid pigment was marked as S-1, and its color parameters of L*, a*, b* were shown in Table 1.

Example 2

(4) 0.3 g of montmorillonite, 0.600 g of iron sulfate and 0.246 g of sodium phosphate were mixed and put into a 45 mL zirconium dioxide ball mill. 36.15 g of 2 mm zirconium dioxide balls with a ball to material ratio of 25 was added and ground at 700 rpm for 60 min, and the obtained precursor was calcined at 600° C. for 90 min. The obtained iron red hybrid pigment was marked as S-2, and its color parameters of L*, a*, b* were shown in Table 1.

Example 3

(5) 0.4 g of sepiolite, 0.127 g of ferric chloride, 0.152 g of ferrous sulfate and 0.250 g of sodium carbonate were mixed and put into a 80 mL zirconium dioxide ball mill. 37.16 g of 2 mm zirconium dioxide balls with a ball to material ratio of 40 was added and ground at 400 rpm for 120 min, and the obtained precursor was calcined at 500° C. for 120 min. The obtained iron red hybrid pigment was marked as S-3, and its color parameters of L*, a*, b* were shown in Table 1.

Example 4

(6) 0.2 g of kaolinite, 0.242 g of ferric nitrate and 0.168 g of sodium carbonate were mixed and put into a 80 mL zirconium dioxide ball mill. 30.50 g of 2 mm zirconium dioxide balls with a ball to material ratio of 50 was added and ground at 400 rpm for 120 min, and the obtained precursor was calcined at 500° C. for 120 min. The obtained iron red hybrid pigment was marked as S-4, and its color parameters of L*, a*, b* were shown in Table 1.

Example 5

(7) 0.2 g of kaolinite, 0.2 g of halloysite, 0.36 g of ferrous acetate and 0.492 g of sodium carbonate were mixed and put into a 80 mL zirconium dioxide ball mill. 37.56 g of 2 mm zirconium dioxide balls with a ball to material ratio of 30 was added and ground at 800 rpm for 240 min, and the obtained precursor was calcined at 700° C. for 90 min. The obtained iron red hybrid pigment was marked as S-5, and its color parameters of L*, a*, b* were shown in Table 1.

(8) TABLE-US-00001 TABLE 1 CIE-L*a*b* color parameters of the iron red/clay mineral hybrid pigment obtained in the Examples of the present disclosure Samples L* a* b* C* S-1 36.11 31.38 29.89 43.33 S-2 37.4  32.15 30.92 44.61 S-3 36.82 31.45 30.62 43.89 S-4 37.66 31.41 30.18 43.56 S-5 38.4  32.27 31.76 45.28

(9) TABLE-US-00002 TABLE 2 CIE-L*a*b* color parameters of the iron red/clay mineral hybrid pigment disclosureafter being immersed into 1 mol/L hydrochloric acid Samples L* a* b* C* S-1 35.9  30.98 28.89 42.36 S-2 36.65 31.48 30.76 45.00 S-3 31.35 31.16 30.40 43.53 S-4 37.40 31.35 30.41 43.68 S-5 38.37 32.01 31.64 45.00

(10) TABLE-US-00003 TABLE 3 CIE-L*a*b* color parameters of the iron red/clay mineral hybrid pigment after being calcined at 900° C. for 2 h Samples L* a* b* C* S-1 33.89 30.18 28.19 41.30 S-2 33.57 30.05 29.32 41.98 S-3 35.44 29.91 30.48 42.80 S-4 34.76 30.56 29.88 42.74 S-5 36.64 31.48 31.06 44.22