CN113149635B - Environment-friendly inorganic pigment and preparation process thereof - Google Patents
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Abstract
The invention belongs to the technical field of inorganic pigments, and particularly relates to an environment-friendly inorganic pigment and a preparation process thereof. The invention is as describedThe environment-friendly inorganic pigment is prepared from raw materials of titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, wherein the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 . The preparation process of the environment-friendly inorganic pigment comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then performing ball milling, then roasting at 1250-1300 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment. The environment-friendly inorganic pigment disclosed by the invention has the advantages that the titanium dioxide, the nickel carbonate, the cobalt carbonate and the rare earth cerium oxide are cooperatively matched, and the mineralizer is added to reduce the calcination temperature to about 1300 ℃, so that the energy consumption is reduced, and the prepared inorganic pigment has stable property, good covering power and good tinting strength.
Description
Technical Field
The invention belongs to the technical field of inorganic pigments, and particularly relates to an environment-friendly inorganic pigment and a preparation process thereof.
Background
Traditional pigments are classified into organic color pastes and inorganic pigments. The organic color paste is prepared by chemical reaction between organic materials or between organic materials and inorganic materials, usually produces many toxic byproducts (waste liquid, waste residue, waste gas and the like), brings certain adverse effects to the living, working and learning environments of human beings, is easy to damage the health of people and the growth of other organisms, causes ecological imbalance and seriously pollutes the environment. Inorganic pigments are oxides of nonferrous metals or some metal-insoluble metal salts, and are divided into natural inorganic pigments and artificial inorganic pigments, and the natural inorganic pigments are mineral pigments.
Natural inorganic pigments are mainly produced by calcining or directly crushing (drying) and grinding inorganic mineral aggregates. The artificial inorganic pigment is prepared by calcining or directly crushing (drying) and grinding inorganic mineral aggregate into powder, and then adding a small amount of coloring material for mixing. The use of natural inorganic pigments is highly appreciated because of their green and environmental benefits.
China is a big country for producing traditional inorganic pigments, the research and development of the inorganic pigments and most of products belong to traditional low-grade pigments with low profits, and green and environment-friendly new products with high added value and no toxicity are lacked. Some toxic pigments are still used in China in large quantities, such as chromium-based pigments, lead-chromium yellow pigments, cadmium orange pigments and cadmium red pigments, and harmful bulk pigments cannot be exported. However, these conventional natural inorganic pigments tend to have poor dispersibility and uneven color.
At present, the yellow inorganic pigment mainly comprises lead chrome yellow (lead chromate), zinc chrome yellow (zinc chromate), cadmium yellow (cadmium sulfide), iron yellow (hydrated iron oxide) and the like. The lead chrome yellow (lead chromate) is the most widely used and has the largest yield. However, lead chrome yellow tends to darken under sunlight; the covering power and the tinting strength of the zinc chrome yellow are poorer than those of the lead chrome yellow; the tinting strength and hiding power of cadmium yellow are not as good as those of lead-chromium yellow, the cost is higher, and the application is limited. Meanwhile, lead chrome yellow and cadmium yellow both contain heavy metals, and therefore cannot be used for coloring in some specific fields, and the application range is limited. The development of a safe, environment-friendly and low-cost substance which can replace the yellow inorganic pigment is of great significance.
Disclosure of Invention
The purpose of the invention is: an environmentally friendly inorganic pigment is provided. The prepared inorganic pigment is non-toxic and pollution-free, has excellent physical, chemical and thermal stability, and is an environment-friendly product; the invention also provides a preparation process of the composite material.
The environment-friendly inorganic pigment provided by the invention comprises the raw materials of titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, wherein the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 。
Preferably, the environment-friendly inorganic pigment comprises, by weight, 50-55 parts of titanium dioxide, 5-7 parts of nickel carbonate, 5-10 parts of cobalt carbonate, 12-15 parts of cerium oxide and 2.2-2.7 parts of a mineralizer.
Most preferably, the environment-friendly inorganic pigment comprises, by weight, 55 parts of titanium dioxide, 5 parts of nickel carbonate, 10 parts of cobalt carbonate, 15 parts of cerium oxide and 2.6 parts of a mineralizer.
The preparation process of the environment-friendly inorganic pigment comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250-.
Wherein:
the grain diameter of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started to raise the temperature from room temperature, firstly raises the temperature to 800 ℃ at the temperature raising rate of 8 ℃/min, keeps the temperature for 1-2h, then raises the temperature to 1250 ℃ at the temperature raising rate of 5 ℃/min, keeps the temperature for 2-2.5h, and finally cools to room temperature at the temperature lowering rate of 3 ℃/min for crushing.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 800-1000 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
According to the environment-friendly inorganic pigment, cobalt and nickel transition metal ions interact with rare earth ions to absorb photon energy and generate 3d electronic configuration, nonradiative transition between 4f-4f and 4f-5d electronic energy levels and Charge Transfer Band (CTB) transition between metal and anions, the absorbed energy is radiationless relaxed into a conduction band, and the other function of the rare earth ions is that photons are absorbed between the energy levels and radiation transition is generated, so that the material is colored and emits light.
Compared with the prior art, the invention has the following beneficial effects:
(1) the environment-friendly inorganic pigment disclosed by the invention is non-toxic and safe, has excellent CIE chromaticity, stable physical and chemical properties, good color uniformity and good weather resistance, light resistance, water resistance and heat resistance.
(2) The environment-friendly inorganic pigment disclosed by the invention has the advantages that the titanium dioxide, the nickel carbonate, the cobalt carbonate and the rare earth cerium oxide are cooperatively matched, and the mineralizer is added to reduce the calcination temperature to about 1300 ℃, so that the energy consumption is reduced, and the prepared inorganic pigment has stable property, good covering power and good tinting strength.
(3) The preparation method of the environment-friendly inorganic pigment has the advantages of simple and convenient process, high automation degree, high yield, low requirement on equipment and stable performance of the prepared inorganic pigment.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The environment-friendly inorganic pigment described in this embodiment 1 is prepared from 55 parts by weight of titanium dioxide, 5 parts by weight of nickel carbonate, 10 parts by weight of cobalt carbonate, 15 parts by weight of cerium oxide and 2.6 parts by weight of mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 。
The preparation process of the environment-friendly inorganic pigment described in the embodiment 1 comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, then roasting at 1280 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the grain diameter of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 750 ℃ at the temperature increase rate of 8 ℃/min, the heat preservation is carried out for 1.5h, then the temperature is increased to 1280 ℃ at the temperature increase rate of 5 ℃/min, the heat preservation is carried out for 2.5h, and finally the temperature is cooled to room temperature at the temperature decrease rate of 3 ℃/min for crushing.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 1000 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 2
The environment-friendly inorganic pigment described in this example 2 is prepared from, by weight, 50 parts of titanium dioxide, 5 parts of nickel carbonate, 7 parts of cobalt carbonate, 14 parts of cerium oxide, and 2.3 parts of a mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 。
The preparation process of the environment-friendly inorganic pigment described in the embodiment 2 comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the grain diameter of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 780 ℃ at the temperature increase rate of 8 ℃/min, the temperature is kept for 2h, then the temperature is increased to 1250 ℃ at the temperature increase rate of 5 ℃/min, the temperature is kept for 2h, and finally the mixture is cooled to room temperature at the temperature decrease rate of 3 ℃/min and crushed.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 900 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 3
The environment-friendly inorganic pigment described in this embodiment 3 is prepared from, by weight, 52 parts of titanium dioxide, 6 parts of nickel carbonate, 5 parts of cobalt carbonate, 13 parts of cerium oxide, and 2.4 parts of a mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 。
The preparation process of the environment-friendly inorganic pigment described in this embodiment 3 is as follows: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1270 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is to heat from room temperature, firstly to 730 ℃ at the heating rate of 8 ℃/min, preserving heat for 2h, then to 1270 ℃ at the heating rate of 5 ℃/min, preserving heat for 2.2h, and finally cooling to room temperature at the cooling rate of 3 ℃/min for crushing.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 800 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 4
The environment-friendly inorganic pigment described in this embodiment 4 is prepared from, by weight, 54 parts of titanium dioxide, 7 parts of nickel carbonate, 5 parts of cobalt carbonate, 15 parts of cerium oxide, and 2.5 parts of a mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 。
The preparation process of the environment-friendly inorganic pigment described in this embodiment 4 is as follows: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1300 ℃, cooling to room temperature, and crushing to obtain the environment-friendly inorganic pigment.
Wherein:
the grain diameter of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is to heat from room temperature, firstly to 800 ℃ at the heating rate of 8 ℃/min, preserving heat for 1.5h, then to 1300 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, and finally to cool to room temperature at the cooling rate of 3 ℃/min for crushing.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 900 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Example 5
The environment-friendly inorganic pigment described in this embodiment 5 is prepared from 55 parts by weight of titanium dioxide, 6 parts by weight of nickel carbonate, 10 parts by weight of cobalt carbonate, 15 parts by weight of cerium oxide, and 2.7 parts by weight of a mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 。
The preparation process of the environment-friendly inorganic pigment described in the embodiment 5 comprises the following steps: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1290 ℃, cooling to room temperature, and crushing to prepare the environment-friendly inorganic pigment.
Wherein:
the particle size of the product is controlled to be less than or equal to 400 meshes after ball milling.
The roasting is started from room temperature, the temperature is firstly increased to 780 ℃ at the heating rate of 8 ℃/min, the temperature is kept for 2h, then the temperature is increased to 1290 ℃ at the heating rate of 5 ℃/min, the temperature is kept for 2.5h, and finally the mixture is cooled to room temperature at the cooling rate of 3 ℃/min and crushed.
The roasting atmosphere is inert atmosphere.
The particle size of the obtained environment-friendly inorganic pigment is controlled to be 1000 meshes after the crushing.
The environment-friendly inorganic pigment prepared by the process is a yellow pigment.
Comparative example 1
The inorganic pigment in comparative example 1 is the same as the preparation process of the environment-friendly inorganic pigment in example 1, and has the unique difference that the raw materials of the inorganic pigment are different, and the raw materials of the inorganic pigment in comparative example 1 comprise 55 parts by weight of titanium dioxide, 5 parts by weight of nickel carbonate, 12 parts by weight of cerium oxide and 2.3 parts by weight of mineralizer; the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 . The finally obtained environment-friendly inorganic pigment is a yellow pigment.
Comparative example 2
The inorganic pigment in the comparative example 2 is the same as the preparation process of the environment-friendly inorganic pigment in the example 1, and has the only difference that the raw materials of the inorganic pigment are different, and the raw materials of the inorganic pigment in the comparative example 2 comprise 55 parts by weight of titanium dioxide, 5 parts by weight of nickel carbonate, 10 parts by weight of cobalt carbonate and 2.6 parts by weight of mineralizer; the mineralizer is Li 2 CO 3 (ii) a The finally obtained environment-friendly inorganic pigment is a yellow pigment.
Comparative example 3
The inorganic pigment in the comparative example 3 is the same as the preparation process of the environment-friendly inorganic pigment in the example 1, and has the only difference that the raw materials of the inorganic pigment are different, and the raw materials of the inorganic pigment in the comparative example 3 comprise 55 parts by weight of titanium dioxide, 10 parts by weight of cobalt carbonate, 15 parts by weight of cerium oxide and 2.6 parts by weight of mineralizer; said ceriumThe oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 . The finally obtained environment-friendly inorganic pigment is a yellow pigment.
Comparative example 4
The inorganic pigment of comparative example 4 has the same composition as the raw material of the environment-friendly inorganic pigment of example 1, and the only difference is that the temperature is raised from room temperature, raised to 1200 ℃ at a heating rate of 8 ℃/min, kept for 4h, and then cooled to room temperature at a cooling rate of 3 ℃/min for crushing. The finally obtained environment-friendly inorganic pigment is a yellow pigment.
The inorganic pigments prepared in examples 1 to 5 and comparative examples 1 to 4 were subjected to the performance test, and the results are shown in Table 1 below.
TABLE 1 inorganic pigment Performance test results
Claims (6)
1. An environment-friendly inorganic pigment, which is characterized in that: the raw materials comprise, by weight, 50-55 parts of titanium dioxide, 5-7 parts of nickel carbonate, 5-10 parts of cobalt carbonate, 12-15 parts of cerium oxide and 2.2-2.7 parts of mineralizer, wherein the cerium oxide is cerium dioxide, and the mineralizer is Li 2 CO 3 ；
The preparation process of the environment-friendly inorganic pigment comprises the steps of mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250-;
wherein: the roasting atmosphere is inert atmosphere, the roasting is to start heating from room temperature, firstly to raise the temperature to 800 ℃ at the heating rate of 8 ℃/min, and keep the temperature for 1-2h, then to raise the temperature to 1300 ℃ at the heating rate of 1250 ℃ at the heating rate of 5 ℃/min, and keep the temperature for 2-2.5h, and finally to cool to room temperature at the cooling rate of 3 ℃/min for crushing.
2. The environmentally friendly inorganic pigment of claim 1, wherein: the raw materials comprise, by weight, 55 parts of titanium dioxide, 5 parts of nickel carbonate, 10 parts of cobalt carbonate, 15 parts of cerium oxide and 2.6 parts of mineralizer.
3. A process for preparing the environmentally friendly inorganic pigment according to claim 1, wherein: mixing titanium dioxide, nickel carbonate, cobalt carbonate, cerium oxide and a mineralizer, then carrying out ball milling, roasting at 1250-.
4. The process for preparing an environmentally friendly inorganic pigment according to claim 3, wherein: the grain diameter of the product is controlled to be less than or equal to 400 meshes after ball milling.
5. The process for preparing an environmentally friendly inorganic pigment according to claim 3, wherein: the particle size of the obtained environment-friendly inorganic pigment is controlled to be 800-1000 meshes after the crushing.
6. The process for preparing an environmentally friendly inorganic pigment according to claim 3, wherein: the environment-friendly inorganic pigment prepared by the process is a yellow pigment.
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| US3956007A (en) * | 1975-01-27 | 1976-05-11 | Kewanee Oil Company | Antimony-free yellow pigments and their preparation |
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| CN103642278B (en) * | 2013-11-29 | 2015-07-29 | 深圳清华大学研究院 | There is titanium system environmental-friendly pigment and the preparation method of composite mineralizer |
| CN103788717B (en) * | 2014-01-18 | 2015-12-02 | 南京理工大学 | A kind of coated nacreous mica composite pigment of doped composite oxide and preparation method |
| EP3202858A1 (en) * | 2016-02-02 | 2017-08-09 | Kronos International, Inc. | The preparation of matt paints and printing inks |
| CN108456437A (en) * | 2018-01-03 | 2018-08-28 | 邯郸市马头盛火陶瓷有限公司 | Inorganic pigment and its preparation method and application |
| CN111154295A (en) * | 2020-01-15 | 2020-05-15 | 吉安市中意陶瓷化工有限公司 | Environment-friendly green inorganic pigment and preparation method thereof |
| CN111548653A (en) * | 2020-05-06 | 2020-08-18 | 中国科学院包头稀土研发中心 | Environment-friendly nontoxic rare earth yellow pigment and preparation method thereof |
| CN112126250B (en) * | 2020-09-24 | 2022-05-13 | 中国科学院包头稀土研发中心 | Rare earth green pigment without cobalt and chromium, and preparation method and application thereof |
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